Fmoc-Ser(tBu)-OH CAS 71989-33-8 Fmoc-O-tert-Butyl-L-Serine Purity >98.5% (HPLC)

Nga tikanga tirotiro
1. Te ahua
-- Te tirotiro tirohanga
2. Pure (HPLC)
2.1 Taputapu
Ko te chromatography wai mahi teitei, te kaitirotiro PDA.
Taurite tātari hiko
2.2 Reagent
Acetonitrile (koeke chromatographic), waikawa trifluoroacetic (koeke chromatographic)
2.3 Nga tikanga Chromatographic
2.3.1 Tīwae: YMC-ODS-AM, 5 μl, 250x4.6 mm
2.3.2 Te roangaru rapu: INC220nm
Rere rere: 1.0mL/min
Rahi tauira:10 μl (tohutoro)
Whakarewa: acetonitrile
Te wa kohikohi raraunga: 25.00min
2.4 Whakaritenga wahanga pūkoro
Waahanga pūkoro A (0.1% te wai waikawa trifluoroacetic): te whakauru tika 2. Whakakorehia te waikawa trifluoroacetic Oml ki te wai ki te 2000m1, uru pai, me te whakaheke;
Wāhanga pūkoro B (0.1% acetonitrile trifluoroacetic acid): te absorption pū 2.0ml waikawa trifluoroacetic i diluted ki te 2000m1 me te acetonitrile, te whakauru me te whakaheke;
2.5 Hōtaka rōnaki o te wā pūkoro
Wā (min) A% B%
0.00 90 10
13.00 10 90
18.00 10 90
18.01 90 10
23.00 90 10
2.6 Te whakarite tauira otinga
Paunatia me te whakakore i te tauira 0.1g me te acetonitrile ka waimeha ki te 100ml, ruru pai hei whakamahi, kia rite ranei te kukū.Whakaritea kia rua nga tauira hei whakarara.
2.7 Tauira Whakatau
Tātarihia te tauira kia rite ki te tikanga tauira e whai ake nei:
Neke atu i te 1 werohanga o te otinga patea
1 tuitui tauira otinga 1#
1 tuitui tauira otinga 2#
2.8 Te tataunga hua
2.8.1 I whakamahia te tikanga whakatikatika rohe tihi ki te tatau i te pokekore o te HPLC ma te tango i te waahi tuwhera.
2.8.2 Kia kaua e nui ake i te 1% te rereketanga o te parakore o nga ngira e rua.
2.8.3 Mena ka tutuki nga hua o nga werohanga e rua ki nga paearu whakaae, ka riro te maatanga toharite hei hua whakamutunga.
3, Ira whakarewa -- RY-1 taputapu ira whakarewa
4. Ngaronga i runga i te whakamaroke tikanga rapunga
4.1 Taputapu:
Umu whakamaroke thermostatic hiko, kotahi i roto i te tekau mano toenga.
4.2 Tikanga:
I roto i te pounamu pauna me te taupoki waha whenua me te taumaha tonu me te whakamaroke nui, paunatia te 1 karamu o te tauira (tika ki te 0.0001 karamu).Ko te tauira kia horahia ki raro o te pounamu pauna me te matotoru kaua e neke atu i te 10mm, ka maka ki roto i te oumu whakamaroke hiko i te pāmahana, whakamaroke i te 105-110 ℃ mo te 3 haora, ka neke ki roto i te ruma whakamaroke, whakamatao. ki te pāmahana rūma me te pauna.
Tātaitanga: Te mate taimaha maroke %= (M1-M2) ÷M×100
Kei hea: M1: te papatipu tauira me te pounamu pauna i mua i te whakamaroke, g
M2: Te papatipu tauira me te pounamu pauna i muri i te whakamaroketanga, g
M: Tauira papatipu, karamu
5. Te hurihanga motuhake
-- Ka inehia te hurihanga motuhake i runga i te GB/T613-1988
Te whakarite tauira: Ko te 0.5000g o te tauira i pauna tika, ka whakawhitia ki te pounamu volumetric 50ml me te maroke me te 20ml Ethyl acetate.I purua te pounamu ka ruia kia memeha te Ethyl acetate.
Whakamātautau: Whakaritea te kore o te gyroscope i mua i te whakamatautau, ka whakakiia te ipuipu whakamatautau ki te tauira otinga, tuhia te koki whakahurihuri, ka tatau i te hurihanga motuhake o te tauira ma te whakamahi i te tauira e whai ake nei.
[α]20/D= (r×50) ÷(L×W)
Kei hea:
[α]20/D: Te hurihanga motuhake o te otinga tauira i te 25 ℃
r: Ka kitea te hurihanga i te 25 ℃ mo te otinga tauira
50: Whakaritehia te tauira otinga rōrahi (ml)
w: Tauira taumaha (g)
L: Roa ngongo whatu (dm)
6. TCL Analysis
Te whakarite tauira: 0.5000g tauira i ata paunatia, ka nekehia ki te pounamu volumetric 50ml ma, maroke, 40ml EtoH i tapirihia, ka kapi te pounamu ka ruia kia memeha, katahi ka diluted ki te tauine ki te EtoH.
Te Whakaritenga o te tauira whakahaere: 0.5000g tauira i ata paunatia, ka nekehia ki te pounamu volumetric 50ml ma, maroke, 40ml wai me te 2 pata o te 6N waikawa pūhaumāota i tāpirihia, ka kapi te pounamu ka ruia kia memeha, ka diluted ki te tauine. wai.Na ka tango i te 0.5 o te wai o runga ake nei ka waimeha ki te waihano i roto i te pounamu rōrahi 100ml ki te tauira tohutoro me te 1.0% te tauine toenga waikawa amino.
10 nga tauira microliter i tangohia me te syringe microsampling, ka tukuna nga tauira ki te pereti silicone GF254.5 microliter, 10 microliter me te 15 microliter point plates i tangohia mo nga tohu whakataurite.
Kaipupuri whakawhanake: n-butanol: waikawa acetic glacial: wai =4:1:1.
Te kaihoko whakawhanake tae: 5% wairewa methanol ninhydrin.
Te mahi whanaketanga tae: tuatahi, whakamahia he whakamaroke makawe hei whakamaroke i te pereti gel silica kua whakawhanakehia, ka toua ki roto ki te wairewa methanol methanol 5% ninhydrin, ka pupuhi maroke, ka tunu i te wera nui i roto i te oumu hiko mo te whanaketanga tae.
Whakawa: Tirohia te wa tae o te hua, te rahi o te waahi, te kukū o te tae me te whakataurite ki te hua whakahaere, whakatauhia kei roto i tera awhe.