1-Methyl-3-Pyrrolidinol CAS 13220-33-2 Purity >98.0% (GC)

Short Description:

Chemical Name: 1-Methyl-3-Pyrrolidinol

Synonyms: 3-Hydroxy-1-Methylpyrrolidine 

CAS: 13220-33-2

Purity: >98.0% (GC)

Appearance: Light Yellow Liquid 

Contact: Dr. Alvin Huang

Mobile/Wechat/WhatsApp: +86-15026746401

E-Mail: alvin@ruifuchem.com


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Description:

Ruifu Chemical is the leading manufacturer of 1-Methyl-3-Pyrrolidinol (3-Hydroxy-1-Methylpyrrolidine) (CAS: 13220-33-2) with high quality. Ruifu Chemical can provide worldwide delivery, competitive price, excellent service, small and bulk quantities available. Purchase 1-Methyl-3-Pyrrolidinol, Please contact: alvin@ruifuchem.com

Chemical Properties:

Chemical Name 1-Methyl-3-Pyrrolidinol 
Synonyms N-Methyl-3-Pyrrolidinol; 3-Hydroxy-1-Methylpyrrolidine; N-Methyl-Pyrrolidin-3-ol; N-Methyl-Pyrrolidinyl Alcohol; 1-Methylpyrrolidin-3-ol
Stock Status In Stock, Commercial Production     
CAS Number 13220-33-2
Molecular Formula C5H11NO
Molecular Weight 101.15 g/mol
Boiling Point 75℃/12 mmHg  
Flash Point 71℃ 
Density 0.921 g/mL at 25℃ (lit.)  
Refractive Index n20/D 1.464(lit.)
Sensitive Air Sensitive, Hygroscopic  
Solubility  Soluble in Water, Soluble in Alcohol, Ether and Benzene 
COA & MSDS Available
Sample  Available
Origin Shanghai, China
Brand Ruifu Chemical

Specifications:

Items Inspection Standards Results
Appearance Light Yellow Liquid  Light Yellow Liquid  
Water by Karl Fischer  <0.20% 0.15% 
Purity / Analysis Method >98.0% (GC)  98.57% 
Density (20℃)  0.920~0.923 Complies 
Refractive Index n20/D 1.463~1.465 Complies 
Infrared Spectrum Consistent with Structure Complies 
1H NMR Spectrum Consistent with Structure Complies 
Conclusion The product has been tested & complies with the given specifications

Package/Storage/Shipping:

Package: Bottle, Aluminium foil bag, 25kg/Cardboard Drum, or according to customer's requirement.

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Storage Condition: Keep the container tightly closed and store in a cool, dry (2~8℃) and well-ventilated warehouse away from incompatible substances. Protect from light and moisture.
Shipping: Deliver to worldwide by air, by FedEx / DHL Express. Provide fast and reliable delivery. 

13220-33-2 - Synthetic Route:

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13220-33-2 - Preparation Method:

Add 1,2,4-Butanetriol and glacial acetic acid to the reaction pot, stir and heat to about 100℃, add dry hydrogen chloride gas, and react at 90~110℃ for 30h, when a large amount of hydrogen chloride began to appear in the tail gas, the end point of the reaction was checked and the hydrogen chloride was stopped. After cooling, the material was discharged, washed with a saturated sodium carbonate solution, and subjected to distillation under reduced pressure, and 120 to 135℃. (12.6 to 13. 3kPa) fraction, I .e., 1,4-Dichloro-2-Butanol oily matter, yield 50%~60%.
Cyclization an aqueous solution of 1,4-Dichloro-2-Butanol and Methylamine was added to the cyclization pot, and heated to 120℃. Under closed heating, and the reaction was stirred for 10h. After cooling, solid sodium hydroxide was added, and the precipitated inorganic salt was filtered off. The oil layer was separated and subjected to vacuum distillation, and the fraction of 76-85℃. (2.1 kPa) was collected to be the finished product. Extraction of the aqueous layer with benzene also yields a portion of 1-Methyl-3-Pyrrolidinol. The yield was about 60%.
3. Key processes:
3.1 Substituted reaction process: control the reaction time and detect the reaction endpoint
3.2 Vacuum distillation process of 1,4-Dichloro-2-Butanol: control vacuum degree of vacuum distillation and fraction temperature
3.3 Cyclization reaction process: control reaction temperature and time
3.4 1-Methyl-3-Pyrrolidinol vacuum distillation process: control vacuum degree of vacuum distillation and fraction temperature
4. Quality control points:
Quality control point 1: 1,2,4-Butanetriol raw material quality standard
Quality control point 2: Central control quality standard for cyclization reaction
Quality control point 3: 1,4-Dichloro-2-Butanol intermediate quality standard
Quality control point 4: 1-Methyl-3-Pyrrolidinol finished product quality standard

13220-33-2 - Test Method:

Moisture Content: Take this product and test it according to the moisture determination method (The First method A of Appendix Ⅷ M, 2010 Edition of the People's Republic of China Pharmacopoeia). The moisture content shall not exceed 0.2%.
Relative Density: The relative density of this product (Appendix VI A of Part II, 2010 edition) is 0.920~0.923
Refractive Index: The refractive index of this product (Appendix VI F of Part II of 2010 edition) is 1.463~1.465
Content Determination: The content of 1-Methyl-3-Pyrrolidinol should not be less than 98.0% by gas chromatography (Appendix Ⅴ E, Part II, 2010 edition).
Column: Capillary in melted silica SPB-5, internal diameter 0.32mm, length 30m
T Injector: 300℃
FID: 320℃
T Column: 80℃ for 5 minutes, to 200℃ at 5℃/min, then at 200℃ for 7 min
Carrier: Helium at 1 ml/min
Split Ratio: 100:1
Injection: 1 microliter
Test solution: dissolve 200mg of the sample under analysis in 10ml of methanol. Inject 1 microliter. 1μl was injected into the gas chromatograph to record the chromatogram. The content of 1-Methyl-3-Pyrrolidinol was calculated by peak area normalization method.  

Advantages:

Sufficient Capacity: Sufficient facilities and technicians

Professional Service: One stop purchasing service

OEM Package: Custom package and label available

Fast Delivery: If within stock, three days delivery guaranteed

Stable Supply: Maintain reasonable stock    

Technical Support: Technology solution available

Custom Synthesis Service: Ranged from grams to kilos

High Quality: Established a complete quality assurance system

FAQ:

How to Purchase? Please contact Dr. Alvin Huang: sales@ruifuchem.com or alvin@ruifuchem.com 

15 Years Experience? We have more than 15 years of experience in the manufacture and export of a wide range of high quality pharmaceutical intermediates or fine chemicals.

Main Markets? Sell to domestic market, North America, Europe, India, Korea, Japanese, Australia, etc.

Advantages? Superior quality, affordable price, professional services and technical support, fast delivery.

Quality AssuranceStrict quality control system. Professional equipment for analysis include NMR, LC-MS, GC, HPLC, ICP-MS, UV, IR, OR, K.F, ROI, LOD, MP, Clarity, Solubility, Microbial limit test, etc.

SamplesMost products provide free samples for quality evaluation, shipping cost should be paid by customers.

Factory AuditFactory audit welcome. Please make an appointment in advance.

MOQ? No MOQ. Small order is acceptable.

Delivery Time? If within stock, three days delivery guaranteed.

TransportationBy Express (FedEx, DHL), by Air, by Sea.

Documents? After sales service: COA, MOA, ROS, MSDS, etc. can be provided.

Custom SynthesisCan provide custom synthesis services to best fit your research needs.

Payment TermsProforma invoice will be sent first after confirmation of order, enclosed our bank information. Payment by T/T (Telex Transfer), PayPal, Western Union, etc. 

13220-33-2 - Risk and Safety:

Hazard Symbols Xi - Irritant
Risk Codes
36/37/38 - Irritating to eyes, respiratory system and skin.
Safety Description
S26 - In case of contact with eyes, rinse immediately with plenty of water and seek medical advice.
S36/37/39 - Wear suitable protective clothing, gloves and eye/face protection.
WGK Germany 3
HS Code 2933990099

13220-33-2 - Application:

1-Methyl-3-Pyrrolidinol (3-Hydroxy-1-Methylpyrrolidine) (CAS: 13220-33-2) is used as an organic synthesis intermediate, used as a pharmaceutical intermediate in the pharmaceutical industry.

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