Ammonia → HCID 14648560, compound

HRID 345150Notes

Reaction equation

HRID 345150 reaction equation
[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[S:21][CH:22]=[CH:23][CH:24]=1.[NH3:25]>CO>[NH2:1][C@@H:2]1[C:8](=[O:9])[N:7]([CH2:10][C:11]([NH2:25])=[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[S:21][CH:22]=[CH:23][CH:24]=1

Participants

4

Reactant 2

HCID 222Ammonia2×HCID 67931189HCID 67931189, compound

Product 1

HCID 14648560HCID 14648560, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

In 300 ml of methanol is dissolved 8 g of ethyl trans-3-amino-4-oxo-2-(2-thienyl)-2,3,4,5-tetrahydro-1,5 -benzothiazepine-5-acetate, and ammonia gas is under ice-cooling blown into the solution until being saturated with ammonia gas. The reaction temperature is slowly elevated to room temperature, and the mixture is left standing for one day. Thereafter, the reaction mixture is concentrated under reduced pressure. Isopropyl alcohol is added to the obtained residue to crystallize. The crystals are collected by filtration to give 7 g of trans-3 amino-4-oxo-2-(2-thienyl)-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide, m.p. 207°-210° C. (decomposition).

Workup

  1. temperaturecooling
  2. customis slowly elevated to room temperature
  3. waitthe mixture is left
  4. concentrationThereafter, the reaction mixture is concentrated under reduced pressure
  5. additionIsopropyl alcohol is added to the obtained residue
  6. customto crystallize
  7. filtrationThe crystals are collected by filtration

Sources & evidence

ORD record
ord-6be1b2f7df0548a784a3e962d3e33f39
Source dataset
uspto-grants-1991_10
Patent number
US05055464

Reaction notes

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