Sodium Carbonate → HCID 20366934、化合物

HRID 617001

反応式

HRID 617001 の反応式
S(C1C=CC(C)=CC=1)(O[CH:5]1[CH2:10][CH2:9][C:8]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)(=O)=[O:2].[Cl:30][C:31]1[CH:36]=[CH:35][C:34]([C:37]2([OH:43])[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)=[CH:33][C:32]=1[C:44]([F:47])([F:46])[F:45].C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1>[OH2:2].[ClH:30].[C:11]1([C:8]2([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[CH2:7][CH2:6][CH:5]([N:40]3[CH2:39][CH2:38][C:37]([C:34]4[CH:35]=[CH:36][C:31]([Cl:30])=[C:32]([C:44]([F:47])([F:45])[F:46])[CH:33]=4)([OH:43])[CH2:42][CH2:41]3)[CH2:10][CH2:9]2)[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 891074-(4-Chloro-3-(trifluoromethyl)phenyl)piperidin-4-olHCID 20366912807-24-9

生成物 1

HCID 20366934HCID 20366934、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 4.1 g of 4,4-diphenylcyclohexyl tosylate, 2.8 g of 4-(4-chloro-3-trifluoromethylphenyl)-4-piperidinol, 1.1 g of sodium carbonate and 400 ml of toluene is stirred under reflux for 48 hours. The reaction mixture is concentrated completely under reduced pressure, water is added to the residue, and the aqueous mixture is extracted with chloroform. The extract is washed with water and dried over sodium sulfate, and the solvent is removed. The esidual viscous oil is purified by column chromatography on silica gel using chloroform and then chloroform - methanol (9:1) as an eluent. The purified base is converted in a conventional manner into the hydrochloride. Thus is obtained 1-(4,4-diphenylcyclohexyl)-4-(4-chloro-3-trifluoromethylphenyl)-4-piperidinol hydrochloride monohydrate as white crystals, melting at 270°-273° C.

後処理

  1. temperatureunder reflux for 48 hours
  2. concentrationThe reaction mixture is concentrated completely under reduced pressure, water
  3. additionis added to the residue
  4. extractionthe aqueous mixture is extracted with chloroform
  5. washThe extract is washed with water
  6. dry with materialdried over sodium sulfate
  7. customthe solvent is removed
  8. customThe esidual viscous oil is purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-6b2e2ad3436c4cc69ba735545e7b983b
出典データセット
uspto-grants-1978_02
特許番号
US04076821

関連ノート

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