Acetyl chloride → 9-Chloro-7-[2-(2,4-di-t-amylphenoxy)butanoylamino]-6-hydroxy-1,5-benzodiazepin-2,4-dione

HRID 1253012

반응식

HRID 1253012 반응식
[NH2:1][C:2]1[C:3]([Cl:32])=[CH:4][C:5]([NH:9][C:10](=[O:31])[CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]([CH2:24][CH3:25])([CH3:23])[CH3:22])=[CH:17][C:16]=2[C:26]([CH2:29][CH3:30])([CH3:28])[CH3:27])[CH2:12][CH3:13])=[C:6]([OH:8])[CH:7]=1.[C:33](Cl)(=[O:35])[CH3:34].C[C:38]([N:40](C)C)=[O:39]>C(#N)C>[Cl:32][C:3]1[C:2]2=[N:1][C:33](=[O:35])[CH2:34][C:38](=[O:39])[N:40]=[C:7]2[C:6]([OH:8])=[C:5]([NH:9][C:10](=[O:31])[CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]([CH2:24][CH3:25])([CH3:23])[CH3:22])=[CH:17][C:16]=2[C:26]([CH2:29][CH3:30])([CH3:28])[CH3:27])[CH2:12][CH3:13])[CH:4]=1

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 31374DimethylacetamideHCID 200361922-{2-(2,4-Di-t-amylphenoxy)butanamido}-4-chloro-5-aminophenol

생성물 1

HCID 1355831249-Chloro-7-[2-(2,4-di-t-amylphenoxy)butanoylamino]-6-hydroxy-1,5-benzodiazepin-2,4-dione

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

In a mixture of 160 ml of acetonitrile and 20 ml of dimethylacetamide was dispersed 40 g of the 5-amino-4-chloro-2-[2-(2,4-di-t-amylphenoxy)butanoylamino]phenol prepared in (1) above, and 6.6 ml of acetyl chloride was added dropwise thereto while refluxing. After stirring while refluxing for 1 hour, the reaction mixture was cooled. The precipitated crystals were collected by filtration and dried to provide 40.8 g of the desired compound.

후처리

  1. temperaturewhile refluxing
  2. temperaturewhile refluxing for 1 hour
  3. temperaturethe reaction mixture was cooled
  4. filtrationThe precipitated crystals were collected by filtration
  5. customdried

출처 및 근거

ORD 기록
ord-2c971836e8e54c8b9d80a884d4a77f43
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04746602

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