Ammonia → trans-3-Amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide

HRID 345143노트

반응식

HRID 345143 반응식
[NH2:1][C@@H:2]1[C:8](=[O:9])[N:7]([CH2:10][C:11]([O:13]CC)=O)[C:6]2[CH:16]=[CH:17][CH:18]=[CH:19][C:5]=2[S:4][C@H:3]1[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.[NH3:26]>CO>[NH2:1][C@@H:2]1[C:8](=[O:9])[N:7]([CH2:10][C:11]([NH2:26])=[O:13])[C:6]2[CH:16]=[CH:17][CH:18]=[CH:19][C:5]=2[S:4][C@H:3]1[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 14648534Ethyl trans-3-amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate

생성물 1

HCID 14648538trans-3-Amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 600 ml of methanol is dissolved 20 g of ethyl trans-3-amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate, into which ammonia gas is blown to the level of saturation under ice-cooling. The reaction temperature is slowly elevated to room temperature, and the mixture is allowed to stand still for 24 hours. Then, the reaction mixture is concentrated under reduced pressure. By adding isopropyl alcohol to the obtained residue, crystallization is effected. The crystals are collected by filtration to give 18 g of trans-3-amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide, m.p. 217°-219° C.

후처리

  1. temperaturecooling
  2. customis slowly elevated to room temperature
  3. concentrationThen, the reaction mixture is concentrated under reduced pressure
  4. additionBy adding isopropyl alcohol
  5. customto the obtained residue, crystallization
  6. filtrationThe crystals are collected by filtration

출처 및 근거

ORD 기록
ord-6b48eddc9d5945a9b371cec852e4480b
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05055464

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