Ammonia → 3-Amino-2-(p-chlorophenyl)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide

HRID 345151노트

반응식

HRID 345151 반응식
[NH2:1][CH:2]1[C:8](=[O:9])[N:7]([CH2:10][C:11](OCC)=[O:12])[C:6]2[CH:16]=[CH:17][CH:18]=[CH:19][C:5]=2[S:4][CH:3]1[C:20]1[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=1.[NH3:27]>CO>[NH2:1][CH:2]1[C:8](=[O:9])[N:7]([CH2:10][C:11]([NH2:27])=[O:12])[C:6]2[CH:16]=[CH:17][CH:18]=[CH:19][C:5]=2[S:4][CH:3]1[C:20]1[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 19993592Ethyl 3-amino-2-(p-chlorophenyl)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate

생성물 1

HCID 146486333-Amino-2-(p-chlorophenyl)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 200 ml of methanol is dissolved 1.5 g of ethyl 3-amino-2-(p-chlorophenyl)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate, and ammonia gas is blown into the solution under ice-cooling up to the saturated state. The reaction temperature is slowly elevated to room temperature, and the reaction mixture is left standing overnight. Then, the reaction mixture is concentrated under reduced pressure. Ethyl acetate is added to the obtained residue, and the resulting crystals are collected by filtration to give 0.9 g of 3-amino-2-(p-chlorophenyl)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide, m.p. 217-220° C. (decomposition).

후처리

  1. temperaturecooling up to the saturated state
  2. customis slowly elevated to room temperature
  3. waitthe reaction mixture is left
  4. concentrationThen, the reaction mixture is concentrated under reduced pressure
  5. additionEthyl acetate is added to the obtained residue
  6. filtrationthe resulting crystals are collected by filtration

출처 및 근거

ORD 기록
ord-c03c649da04a42e48666a8b9e478d508
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05055464

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