Potassium Carbonate → HCID 13500543, compound

HRID 905167Notes

Reaction equation

HRID 905167 reaction equation
Cl.[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:12]2[C:18]3[CH:19]=[C:20]([O:25][CH3:26])[C:21]([O:23][CH3:24])=[CH:22][C:17]=3[CH:16]([CH2:27][CH3:28])[CH:15]([CH3:29])[NH:14][N:13]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH3:11].C(=O)([O-])[O-].[K+].[K+]>O>[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:12]2[C:18]3[CH:19]=[C:20]([O:25][CH3:26])[C:21]([O:23][CH3:24])=[CH:22][C:17]=3[CH:16]([CH2:27][CH3:28])[CH:15]([CH3:29])[NH:14][N:13]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH3:11]

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 20475687HCID 20475687, compound

Product 1

HCID 13500543HCID 13500543, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent3×

Procedure

To a suspension of 42.1 g (0.1 mole) of 1-(3,4-dimethoxyphenyl)-4-methyl-5-ethyl-7,8-dimethoxy-3,4-dihydro-5H-2,3-benzodiazepine hydrochloride in 400 ml of water (or to a solution of the said compound in hot water), 8 g of potassium carbonate are added in small parts. The desired compound separates in form of crystals containing 1 mole of crystal water. The product is filtered off, washed chloride-free five times with 15 ml of water each and dried. 34 g (85%) of the desired compound are obtained. The white crude product shrinks from 75° C., between 105° and 115° C. it forms a bubbly coagulate.

Workup

  1. additionare added in small parts

Sources & evidence

ORD record
ord-a013c84acb974a63ad94ea18ab74598d
Source dataset
uspto-grants-1983_12
Patent number
US04423044

Reaction notes

Loading…