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Benzyl chloroformate → 8alpha-Benzyloxycarbonylamino-6-methylergoline

HRID 34953
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HRID 34953 반응식
[C:1](Cl)([O:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:2].[NH2:12][C@H:13]1[CH2:27][C@H:26]2[C@@H:16]([CH2:17][C:18]3[C:28]4[C:21](=[CH:22][CH:23]=[CH:24][C:25]2=4)[NH:20][CH:19]=3)[N:15]([CH3:29])[CH2:14]1>C(Cl)(Cl)Cl.C(O)(C)C.[OH-].[Na+]>[CH2:4]([O:3][C:1]([NH:12][C@H:13]1[CH2:27][C@H:26]2[C@@H:16]([CH2:17][C:18]3[C:28]4[C:21](=[CH:22][CH:23]=[CH:24][C:25]2=4)[NH:20][CH:19]=3)[N:15]([CH3:29])[CH2:14]1)=[O:2])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 10387Benzyl chloroformateHCID 67752218HCID 67752218, 화합물

생성물 1

HCID 704178488alpha-Benzyloxycarbonylamino-6-methylergoline

시약·촉매·용매 3

HCID 3776Isopropanol용매HCID 6212Chloroform용매HCID 14798Sodium Hydroxide용매

실험 절차

10.5 ml (75 mM) carbobenzyloxychloride are added to a suspension of 18 g (74.7 mM) 8α-amino-6-methylergoline in 1000 ml chloroform, 150 ml isopropanol and 37 ml 2N (74 mM) sodium hydroxide at room temperature. The mixture is stirred for 2 hours at room temperature. After separation of the organic phase, this is dried, filtered and concentrated. The resultant crude product is filtered through silicagel with methylene chloride/methanol (99:1) giving the heading compound as a foam.

후처리

  1. customAfter separation of the organic phase
  2. customthis is dried
  3. filtrationfiltered
  4. concentrationconcentrated
  5. filtrationThe resultant crude product is filtered through silicagel with methylene chloride/methanol (99:1)

출처 및 근거

ORD 기록
ord-3f87fa4d595649339559f8787de76637
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04764517

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