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

HRID 345143

反応式

HRID 345143 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 14648538trans-3-Amino-4-oxo-2-phenyl-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 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.

後処理

  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

出典と根拠

ORDレコード
ord-6b48eddc9d5945a9b371cec852e4480b
出典データセット
uspto-grants-1991_10
特許番号
US05055464

関連ノート

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