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Z-Sta-Ala-OC(CH3)3 → Z-Sta-Ala-OH

HRID 1982321
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HRID 1982321 반응식
[NH:1]([C:22]([O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:23])[C@H:2]([C@H:7]([CH2:9][C:10]([NH:12][C@H:13]([C:15]([O:17]C(C)(C)C)=[O:16])[CH3:14])=[O:11])[OH:8])[CH2:3][CH:4]([CH3:6])[CH3:5]>FC(F)(F)C(O)=O>[NH:1]([C:22]([O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:23])[C@H:2]([C@H:7]([CH2:9][C:10]([NH:12][C@H:13]([C:15]([OH:17])=[O:16])[CH3:14])=[O:11])[OH:8])[CH2:3][CH:4]([CH3:6])[CH3:5]
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참가 물질

3

반응물 1

HCID 131714736Z-Sta-Ala-OC(CH3)3

생성물 1

HCID 131714737Z-Sta-Ala-OH

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

반응 조건

온도
25 °C

실험 절차

470 mg of Z-Sta-Ala-OC(CH3)3 (from stage 13.1) are dissolved in 10 ml of trifluoroacetic acid and the solution is stirred for 10 minutes at 25° C. The solvent is then removed in a rotary evaporator and the residue is flash-chromatographed over 200 g of silica gel (eluant first chloroform/methanol/concentrated aqueous ammonia solution [40:10:1], then chloroform/methanol/concentrated aqueous ammonia solution [5:3:1]). The product-containing fractions are combined and concentrated by evaporation, the residue is taken up in chloroform and the chloroform solution is extracted with dilute hydrochloric acid and saturated sodium chloride solution, dried and concentrated by evaporation. After drying the residue in a high vacuum, Z-Sta-Ala-OH is obtained in the form of a colourless foam; Rf (G)=0.43.

후처리

  1. customThe solvent is then removed in a rotary evaporator
  2. customthe residue is flash-chromatographed over 200 g of silica gel (eluant first chloroform/methanol/concentrated aqueous ammonia solution [40:10:1]
  3. concentrationconcentrated by evaporation
  4. extractionthe chloroform solution is extracted with dilute hydrochloric acid and saturated sodium chloride solution
  5. customdried
  6. concentrationconcentrated by evaporation
  7. customAfter drying the residue in a high vacuum

출처 및 근거

ORD 기록
ord-e851fdd31e504198a633ac0f33e12bde
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04595677

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