4-Amino-5-Chloro-2,3-Dihydrobenzofuran-7-Carboxylic Acid CAS 123654-26-2 Prucalopride Succinate Intermediate Maʻemaʻe ≥98.0% (HPLC)

ʻO kēia huahana he 4-Amino-5-Chloro-2,3-Dihydrobenzofuran-7-Carboxylic Acid, ʻaʻole e emi iho ka ʻike o C12H12ClNO4 ma mua o 98.0%, helu ʻia ma ke kumu anhydrous.
[Properties] He keʻokeʻo keʻokeʻo a ʻulaʻula māmā kēia huahana.
[Holo]
E lawe i ka nui kūpono o kēia huahana (ma kahi o 0.5g) o ka wai, e hoʻohui i ka solvent (methanol: N,N-dimethylformamide = 50:50), a e hoʻoheheʻe ʻia e like me ke ʻano o ka hoʻoholo ʻana i ka wai (Appendix Ⅷ M, ka hana mua A).E hoʻohana i nā hāʻule hoʻāʻo a Fisher e hoʻoholo ai a hiki i ka hoʻololi ʻana o ka hopena mai ka melemele māmā a i ka ʻulaʻula-ʻulaʻula e hōʻike ana i ka hopena, a e hana i kahi hoʻāʻo ʻē aʻe.E helu e like me kēia ʻano: ʻaʻole pono ka nui o ka wai ma mua o 1.00%.
ʻO ka ʻoluʻolu (%) = (AB) F/W×100%
Aia, ʻo A ka nui o ka wai a Fisher i hoʻopau ʻia e ka huahana hoʻāʻo (ml);
ʻO B ka nui o ka wai hoʻāʻo a Fisher i hoʻopau ʻia e kahi hakahaka, ml;
ʻO F ke kaumaha o ka hopena hoʻāʻo a Fisher e like me ka wai no 1ml, mg;
ʻO W ke kaumaha o ka huahana hoʻāʻo, mg
Mea pili
E like me ke ʻano ma lalo o ka "mea ana maʻiʻo", inā he mau piko haumia i loko o ka chromatogram o ka hopena hoʻāʻo, ʻaʻole ʻoi aku ka nui o ka wahi kiʻekiʻe o kahi haumia hoʻokahi ma mua o 10 mau manawa (1.0%) o ka wahi kiʻekiʻe o ka mana. ʻAʻole ʻoi aku ka nui o ka huina o ka wahi kiʻekiʻe o nā haumia a pau ma mua o 20 manawa (2.0%) o ka ʻāpana kiʻekiʻe o ka hopena hoʻomalu.
[Ka Hoʻoholo Manaʻo] E like me ka chromatography wai kiʻekiʻe (Appendix VI D).
Ua hoʻohana ʻia ʻo Octadecylsilane bonded silica gel i mea hoʻopiha no nā kūlana chromatographic a me nā hoʻāʻo kūpono o ka ʻōnaehana.Phosphate buffer solution (1.36g potassium dihydrogen phosphate, dissolved ultrasonic in 1L wai, phosphoric acid i hoʻololi ʻia i ka PH 3.0) ua hoʻohana ʻia e like me ka mobile phase A. ʻO ka Acetonitrile ka pae B, a ua hana ʻia ka gradient elution e like me ka papa ma lalo:
Manawa (min) Māhele paʻalima A pae paʻa paʻa B
0 80 20
15 80 20
30 50 50
45 50 50
ʻO 254 nm ka lōʻihi nalu.ʻO 1.0 ml / min ka kahe kahe.ʻAʻole emi ka helu o nā papa theoretical ma mua o 2000 e like me ka piko o 4-Amino-5-Chloro-2,3-Dihydrobenzofuran-7-Carboxylic Acid.
ʻAʻole emi ka piko o ka waikawa furanoformic ma mua o 2000.
ʻano hoʻoholo:
E lawe i 10mg o ka huahana ho'āʻo, e kaupaona pololei, e hoʻokomo i loko o A 10ml omole, e hoʻoheheʻe i kani ultrasonic me ka mobile phase A-mobile phase B (70:30) e like me ka solvent, dilute ia i ka unahi, lulu maikaʻi, a hoʻomākaukau i kahi. ka hoʻonā me ka manaʻo o 1mg / ml.Ua hoʻokomo ʻia ka 20 l o ka pololei i loko o ka chromatograph wai, a ua hoʻopaʻa ʻia ka chromatogram.ʻAʻole i emi iho ka maʻemaʻe kiʻekiʻe ma mua o 98.0% e like me ke ʻano maʻamau maʻamau
Kona: Dionex Acclaim C18, 4.6*250mm, 5um
Ka wela o ke kolamu: 40 ℃
Kahe kahe: 1.0ml / min
Ka lōʻihi nalu ʻike: 254nm
Laʻana nui: 10μL