Hydrochloric Acid → 1-Cyclohexyl-4-[4-(2-methoxy-phenyl)-piperazin-1-YL]-2-phenyl-butan-1-one dihydrochloride

HRID 277752

반응식

HRID 277752 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][C:17]([C:25]([CH:27]2[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]2)=[O:26])([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH3:18])[CH2:11][CH2:10]1.[ClH:33].C(OCC)C>CO>[ClH:33].[ClH:33].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][C:17]([C:25]([CH:27]2[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]2)=[O:26])([C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH3:18])[CH2:13][CH2:14]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 98029871-Cyclohexyl-4-(4-(2-methoxyphenyl)piperazin-1-yl)-2-methyl-2-phenylbutan-1-one

생성물 1

HCID 222441101-Cyclohexyl-4-[4-(2-methoxy-phenyl)-piperazin-1-YL]-2-phenyl-butan-1-one dihydrochloride수율 76%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

(+)-1-(2-methoxyphenyl)-4-[3-(cyclohexanecarbonyl)-3-(phenyl)butyl]piperazine (15.0 g, 34.5 mmol, prepared above) was diluted with methanol (40 30 mL). To this solution was added HCl (9.58 g of a 26.3% solution in methanol, 69.0 mmol). The mixture began to form gelatinous-looking crystals and set up solid within minutes. To this mixture was added with vigorous stirring, diethyl ether (100 mL). The white solid was collected by suction filtration and then dried under vacuum at 450° C. for two days to provide the title compound (13.4 g, 76%) as a white solid; mp(DSC)=195.58° C.

후처리

  1. customto form gelatinous-looking crystals
  2. filtrationThe white solid was collected by suction filtration
  3. customdried under vacuum at 450° C. for two days

출처 및 근거

ORD 기록
ord-4b80ac507948482482a87a08475e7be8
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06358958B2

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