Ammonia → HCID 14648596, compound

HRID 345158Notes

Reaction equation

HRID 345158 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 14648593HCID 14648593, compound

Product 1

HCID 14648596HCID 14648596, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

In the same manner as in (iv) of Example 23, 1.7 g of ethyl trans-3-amino-8-chloro-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate is dissolved in 50 ml of methanol, 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 1.4 g of trans-3-amino-8-chloro-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide, m.p. 225°-228° C.

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-4526f9b7f3d84dc5918ed1a954d22636
Source dataset
uspto-grants-1991_10
Patent number
US05055464

Reaction notes

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