Ammonia → HCID 14648630, compound

HRID 345148Notes

Reaction equation

HRID 345148 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH:15]([NH:16][C:17]([C:19]3[CH:28]=[CH:27][C:26]4[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=4)[CH:20]=3)=[O:18])[C:14](=[O:29])[N:13]([CH2:30][C:31]([O:33]CC)=O)[C:12]3[CH:36]=[CH:37][CH:38]=[CH:39][C:11]=3[S:10]2)=[CH:5][CH:4]=1.[NH3:40]>CO>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH:9]2[CH:15]([NH:16][C:17]([C:19]3[CH:28]=[CH:27][C:26]4[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=4)[CH:20]=3)=[O:18])[C:14](=[O:29])[N:13]([CH2:30][C:31]([NH2:40])=[O:33])[C:12]3[CH:36]=[CH:37][CH:38]=[CH:39][C:11]=3[S:10]2)=[CH:7][CH:8]=1

Participants

4

Reactant 2

HCID 222AmmoniaHCID 14648629HCID 14648629, compound

Product 1

HCID 14648630HCID 14648630, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

In 500 ml of methanol is dissolved 1.8 g of ethyl 2-p-methoxyphenyl- 3-(2-naphthalenecarboxamido)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate, into which ammonia gas is blown under ice-cooling for about 1 hour. After the mixture is allowed to stand still at room temperature for 3 days, the reaction mixture is concentrated under reduced pressure to the volume of about 50 ml to give crystals. The crystals are collected by filtration to give 1.2 g of 2-p-methoxyphenyl-3-(2-naphthalenecarboxamido)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide, m.p. 243°-245° C.

Workup

  1. temperaturecooling for about 1 hour
  2. concentrationthe reaction mixture is concentrated under reduced pressure to the volume of about 50 ml
  3. customto give crystals
  4. filtrationThe crystals are collected by filtration

Sources & evidence

ORD record
ord-eb199a5d97f541bdba37eff3809f3d64
Source dataset
uspto-grants-1991_10
Patent number
US05055464

Reaction notes

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