Ammonia → HCID 67931168, compound

HRID 345157Notes

Reaction equation

HRID 345157 reaction equation
[NH2:1][C@H:2]1[C:8](=[O:9])[N:7]([CH2:10][C:11](OCC)=[O:12])[C:6]2[CH:16]=[CH:17][C:18]([Cl:20])=[CH:19][C:5]=2[S:4][C@H:3]1[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[NH3:27]>CO>[NH2:1][C@H:2]1[C:8](=[O:9])[N:7]([CH2:10][C:11]([NH2:27])=[O:12])[C:6]2[CH:16]=[CH:17][C:18]([Cl:20])=[CH:19][C:5]=2[S:4][C@H:3]1[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

Participants

4

Reactant 2

HCID 222AmmoniaHCID 67931341HCID 67931341, compound

Product 1

HCID 67931168HCID 67931168, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

In 220 ml of methanol is dissolved 6.9 g of ethyl cis-3-amino-8-chloro-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 overnight. Then, the reaction mixture is concentrated under reduced pressure. The separated crystals are collected by filtration to give 6.2 g of cis-3-amino-8-chloro-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide.

Workup

  1. temperaturecooling
  2. customis slowly elevated to room temperature
  3. concentrationThen, the reaction mixture is concentrated under reduced pressure
  4. filtrationThe separated crystals are collected by filtration

Sources & evidence

ORD record
ord-74bd00e3258448ceb529b87b36b79eb7
Source dataset
uspto-grants-1991_10
Patent number
US05055464

Reaction notes

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