Dichloromethane → HCID 14748687, compound

HRID 1709302Notes

Reaction equation

HRID 1709302 reaction equation
[C:1]1([CH:7]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][NH2:17])[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.C(Cl)Cl.[C:34]1([S:40](Cl)(=[O:42])=[O:41])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1>C(Cl)(Cl)Cl>[C:18]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[N:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][NH:17][S:40]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)(=[O:42])=[O:41])[CH2:12][CH2:13]2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 7369Benzenesulfonyl chlorideHCID 8471TriethylamineHCID 137677783-(4-Benzhydryl-1-piperazinyl)-1-propanamine

Product 1

HCID 14748687HCID 14748687, compoundYield 114.7%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

85 mg of 1-diphenylmethyl-4-(3-aminopropyl)-piperazine and 102.5 mg of triethylamine were added to ml of methylene chloride, and under ice cooling and stirring, 39.4 mg of benzenesulfonyl chloride was added. The mixture was further stirred at this temperature for 1 hour. Chloroform was added to the reaction mixture, and the mixture was washed with water and dried. The solvent was then evaporated to give 115 mg of the captioned compound as a crude product. It was converted to a dihydrochloride in a customary manner, and recrystallization from ethanol/ether gave 92.7 mg of the captioned compound as a colorless powdery crystal having a melting point of 160° to 165° C. (decomp.). ##STR4##

Workup

  1. stirringThe mixture was further stirred at this temperature for 1 hour
  2. washthe mixture was washed with water
  3. customdried
  4. customThe solvent was then evaporated

Sources & evidence

ORD record
ord-2bf71c496629402e9c8b248bd36946c8
Source dataset
uspto-grants-1990_08
Patent number
US04948892

Reaction notes

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