alpha,alpha-Bis(3-methoxyphenyl)-4-piperidineethanol → 4-[2,2-Bis(3-methoxyphenyl)ethenyl]piperidine

HRID 1249586노트

반응식

HRID 1249586 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:9]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([O:24][CH3:25])[CH:19]=2)(O)[CH2:10][CH:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[CH:6]=[CH:7][CH:8]=1>FC(F)(F)C(O)=O>[CH3:25][O:24][C:20]1[CH:19]=[C:18]([C:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=2)=[CH:10][CH:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[CH:23]=[CH:22][CH:21]=1

참가 물질

3

반응물 1

HCID 13754499alpha,alpha-Bis(3-methoxyphenyl)-4-piperidineethanol

생성물 1

HCID 137545014-[2,2-Bis(3-methoxyphenyl)ethenyl]piperidine수율 90.1%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of alpha,alpha-bis(3-methoxyphenyl)-4-piperidine-ethanol (15 g) in trifluoroacetic acid (30 ml) was stirred at ambient temperature for one hour, then the solvent was removed in vacuo. The residue was partitioned between toluene (50 ml) and 1N sodium hydroxide (100 ml), and the separated aqueous layer was reextracted with toluene (20 ml). The combined toluene extracts were washed with 1N sodium hydroxide solution, then were dried over potassium carbonate and evaporated to give 12.8 g of 4-[2,2-bis(3-methoxyphenyl)ethenyl]piperidine as an oil.

후처리

  1. customthe solvent was removed in vacuo
  2. customThe residue was partitioned between toluene (50 ml) and 1N sodium hydroxide (100 ml)
  3. washThe combined toluene extracts were washed with 1N sodium hydroxide solution
  4. dry with materialwere dried over potassium carbonate
  5. customevaporated

출처 및 근거

ORD 기록
ord-75360393f5b3463fa3fb2d8db2f696c3
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04632925

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