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

HRID 2789노트

반응식

HRID 2789 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6084487d99d546f3b8c77a5c36cc747e
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731331

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