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Hydrochloric Acid → 4-[2,2-Bis(4-fluorophenyl)ethyl]piperidine hydrochloride hydrate

HRID 1709855
ノート
印刷プレビュー

反応式

HRID 1709855 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)([OH:16])[CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.[H][H].[ClH:26].CCOCC>[Pt].CC(OCC1C2C(=CC=CC=2)C(COC(C)=O)=C2C=1C=CC=C2)=O.CO>[OH2:16].[ClH:26].[F:23][C:20]1[CH:21]=[CH:22][C:17]([CH:8]([C:5]2[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=2)[CH2:9][CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:18][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 15020359alpha,alpha-Bis(4-fluorophenyl)-4-pyridineethanolHCID 178418361HCID 178418361、化合物

生成物 1

HCID 199831054-[2,2-Bis(4-fluorophenyl)ethyl]piperidine hydrochloride hydrate

試薬・触媒・溶媒 3

HCID 23939Platinum
触媒
HCID 887Methanol溶媒
HCID 613145Acetic acid 10-acetoxymethyl-anthracen-9-ylmethyl ester溶媒

実験手順

A mixture of 10.0 g (0.30 mole) α,α-bis(4-fluoropheny)-4-pyridineethanol of 1.2 g of 5% platinum on carbon catalyst in 200 ml of acetic and was shaken under an atomsphere of hydrogen (49 psi)for 16 hr. The solution was filtered through Celite®, and the solvent was removed in vacuo. The residue was partitioned between methylene chloride and dilute sodium hydroxide. The solvent was removed in vacuo to give an oil. This was dissolved in methanol, an excess of ethereal hydrogen chloride was added and ether was added. A precipitate was collected to give 7.58 g (72.4%)as a white, crystalline solid, m.p. 171°-173° C.

後処理

  1. filtrationThe solution was filtered through Celite®
  2. customthe solvent was removed in vacuo
  3. customThe residue was partitioned between methylene chloride and dilute sodium hydroxide
  4. customThe solvent was removed in vacuo
  5. customto give an oil
  6. customA precipitate was collected
  7. customto give 7.58 g (72.4%)as a white, crystalline solid, m.p. 171°-173° C.

出典と根拠

ORDレコード
ord-24d604a3540e401485aab46c83fd1feb
出典データセット
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04950674

反応ノート

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