Hydrochloric Acid → 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone Hydrochloride

HRID 1840588노트

반응식

HRID 1840588 반응식
[N:1]1([CH2:6][C:7]2[CH:12]=[CH:11][C:10]([S:13]([N:16]3[CH2:21][CH2:20][N:19]([CH2:22][CH:23]4[CH2:28][CH2:27][N:26]([C:29]5[CH:34]=[CH:33][N:32]=[CH:31][CH:30]=5)[CH2:25][CH2:24]4)[C:18](=[O:35])[CH2:17]3)(=[O:15])=[O:14])=[CH:9][CH:8]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.[ClH:36]>C(OCC)(=O)C>[ClH:36].[N:1]1([CH2:6][C:7]2[CH:8]=[CH:9][C:10]([S:13]([N:16]3[CH2:21][CH2:20][N:19]([CH2:22][CH:23]4[CH2:28][CH2:27][N:26]([C:29]5[CH:30]=[CH:31][N:32]=[CH:33][CH:34]=5)[CH2:25][CH2:24]4)[C:18](=[O:35])[CH2:17]3)(=[O:14])=[O:15])=[CH:11][CH:12]=2)[CH:5]=[CH:4][N:3]=[CH:2]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 234475814-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone

생성물 1

HCID 234475804-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone Hydrochloride

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A mixture of 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone dihydrochloride (209 mg) and chloropyridine hydrochloride (93 mg) was added to sodium bicarbonate solution, and the mixture was extracted with dichloromethane (twice), dried and concentrated. To the residue was added isoamylalcohol (10 ml), and the mixture was stirred at 130% for 15 hours. The reaction solution was concentrated, and the residue was dissolved in dichloromethane. The solution was washed with 1N sodium hydroxide solution, dried and concentrated, and the residue was purified with silica gel column chromatography (dichloromethane:methanol containing 10% ammonia solution=7:1) to give colorless solid of 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone (102 mg). The obtained 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone was dissolved in ethyl acetate (5 ml), and to the solution was added a solution of 4N hydrochloric acid in ethyl acetate. Precipitates were filtered, washed with ethyl acetate and dried to give colorless solid of the title compound (103 mg).

후처리

  1. customPrecipitates
  2. filtrationwere filtered
  3. washwashed with ethyl acetate
  4. customdried

출처 및 근거

ORD 기록
ord-91851b7837de49c497ae55368b3cb024
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06680312B2

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