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

HRID 1249586ノート

反応式

HRID 1249586 の反応式
[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

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-75360393f5b3463fa3fb2d8db2f696c3
出典データセット
uspto-grants-1986_12
特許番号
US04632925

反応ノート

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