Hydrochloric Acid → 1-[4-(4-phenyl-1,2,3,6-tetrahydro-1-pyridyl)butyl]-1H-benzimidazole

HRID 2789ノート

反応式

HRID 2789 の反応式
O[C:2]1([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][CH2:11][N:12]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[N:14]=[CH:13]2)[CH2:4][CH2:3]1.Cl>C(O)C>[C:21]1([C:2]2[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][CH2:11][N:12]3[C:16]4[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=4[N:14]=[CH:13]3)[CH2:4][CH:3]=2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 154861071-[4-(4-hydroxy-4-phenyl-1-piperidyl)butyl]-1H-benzimidazole

生成物 1

HCID 154861111-[4-(4-phenyl-1,2,3,6-tetrahydro-1-pyridyl)butyl]-1H-benzimidazole収率 72%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 13.4 g (38.2 mmol) of 1-[4-(4-hydroxy-4-phenyl-1-piperidyl)butyl]-1H-benzimidazole, 150 ml of concentrated HCl and 75 ml of ethanol is heated at reflux for 6 hours. The ethanol is then evaporated and the aqueous solution is cooled, basified with dilute NaOH and extracted with chloroform. The organic phase is dried with anhydrous sodium sulfate and evaporated at reduced pressure, a crude product being obtained which is purified by chromatography on silica gel. 9.1 g (27.5 mmol) of 1-[4-(4-phenyl-1,2,3,6-tetrahydro-1-pyridyl)butyl]-1H-benzimidazole are obtained.

後処理

  1. temperatureat reflux for 6 hours
  2. customThe ethanol is then evaporated
  3. temperaturethe aqueous solution is cooled
  4. extractionextracted with chloroform
  5. dry with materialThe organic phase is dried with anhydrous sodium sulfate
  6. customevaporated at reduced pressure
  7. customa crude product being obtained which
  8. customis purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-6084487d99d546f3b8c77a5c36cc747e
出典データセット
uspto-grants-1998_03
特許番号
US05731331

反応ノート

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