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

HRID 432030

反応式

HRID 432030 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

(+)-1-(2-methoxyphenyl)-4-[3-(cyclohexanecarbonyl)-3-(phenyl)butyl]piperazine (15.0 g, 34.5 mmol, prepared above) was diluted with methanol (40 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 45° C. for two days to provide the title compound (13.4 g, 76%) as a white solid; mp(DSC)=195.58° C.

後処理

  1. customto form gelatinous-looking crystals
  2. filtrationThe white solid was collected by suction filtration
  3. customdried under vacuum at 45° C. for two days

出典と根拠

ORDレコード
ord-d54df489598441d9bbf664a5b27d50d7
出典データセット
uspto-grants-2003_12
特許番号
US06660859B2

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