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

HRID 345151ノート

反応式

HRID 345151 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c03c649da04a42e48666a8b9e478d508
出典データセット
uspto-grants-1991_10
特許番号
US05055464

反応ノート

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