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Acetic Acid → 4-[Bis(4-fluorophenyl)methylene]-1-(phenylmethyl)piperidine

HRID 484715
ノート
印刷プレビュー

反応式

HRID 484715 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)([CH:10]2[CH2:15][CH2:14][N:13]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:12][CH2:11]2)O)=[CH:4][CH:3]=1.Cl.C(O)(=O)C.O>CC1C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:23]2[CH:24]=[CH:25][C:26]([F:29])=[CH:27][CH:28]=2)=[C:10]2[CH2:15][CH2:14][N:13]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:12][CH2:11]2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 962WaterHCID 13519964alpha,alpha-Bis(4-fluorophenyl)-1-(phenylmethyl)-4-piperidinemethanol

生成物 1

HCID 135199654-[Bis(4-fluorophenyl)methylene]-1-(phenylmethyl)piperidine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 40 parts of α,α-bis(4-fluorophenyl)-1-(phenylmethyl)-4-piperidinemethanol, 120 parts of a hydrochloric acid solution and 50 parts of acetic acid was stirred and refluxed for 2 hours. The reaction mixture was cooled and water and methylbenzene were added: three layers were obtained. The two supernatant phases were separated and treated with ammonium hydroxide. The organic phase was separated, dried, filtered and evaporated. The residue was crystallized from 2,2'-oxybispropane, yielding 26 parts of 4-[bis(4-fluorophenyl)methylene]-1-(phenylmethyl)piperidine (intermediate 13).

後処理

  1. temperaturerefluxed for 2 hours
  2. temperatureThe reaction mixture was cooled
  3. customthree layers were obtained
  4. customThe two supernatant phases were separated
  5. additiontreated with ammonium hydroxide
  6. customThe organic phase was separated
  7. customdried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue was crystallized from 2,2'-oxybispropane

出典と根拠

ORDレコード
ord-74ff45c5dba744e4994864b4ca504911
出典データセット
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04533665

反応ノート

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