Pyridine → HCID 21431624, compound

HRID 436893Notes

Reaction equation

HRID 436893 reaction equation
[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[C:6]3[NH:20][N:19]=[CH:18][C:7]=3[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1.Cl[C:24]([O:26][CH2:27][CH3:28])=[O:25].N1C=CC=CC=1.C(Cl)Cl>C(Cl)(Cl)Cl>[ClH:1].[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[C:6]3[C:7](=[CH:18][N:19]([C:24]([O:26][CH2:27][CH3:28])=[O:25])[N:20]=3)[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1

Participants

6

Reactant 4

HCID 1049PyridineHCID 6344DichloromethaneHCID 10928Ethyl chloroformateHCID 20321571HCID 20321571, compound

Product 1

HCID 21431624HCID 21431624, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

The mixture of 0.33 g of 8-chloro-6-(2-chlorophenyl)-1H,4H-pyrazolo[4,3-d](2)benzazepine, 0.141 g of ethyl chloroformate, 0.16 g of pyridine and 10 ml of methylene chloride is stirred at room temperature for 2 hours. It is diluted with chloroform, washed with aqueous sodium bicarbonate, the organic phase separated, dried and evaporated. The residue is taken up in the minimum amount of acetone and the solution neutralized with ethereal hydrogen chloride, to yield the 8-chloro-6-(2-chlorophenyl)-2 -ethoxycarbonyl-2H,4H-pyrazolo[4,3-d](2)benzazepine hydrochloride melting at 151°-152°.

Workup

  1. washwashed with aqueous sodium bicarbonate
  2. customthe organic phase separated
  3. customdried
  4. customevaporated

Sources & evidence

ORD record
ord-fb760b4683e844acaa1a73c2f27cb727
Source dataset
uspto-grants-1977_06
Patent number
US04028381

Reaction notes

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