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Water → HCID 19992280、化合物

HRID 345487
ノート
印刷プレビュー

反応式

HRID 345487 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)([CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[OH:9])=[CH:4][CH:3]=1.Cl[CH2:24][CH2:25][C:26]([N:28]([CH3:30])[CH3:29])=[O:27].C(=O)([O-])[O-].[Na+].[Na+].O>CN(C)C=O.[I-].[K+]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:17]=[CH:18][C:19]([F:22])=[CH:20][CH:21]=2)([OH:9])[CH:10]2[CH2:11][CH2:12][N:13]([CH2:24][CH2:25][C:26]([N:28]([CH3:30])[CH3:29])=[O:27])[CH2:14][CH2:15]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

7

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 32690663-chloro-N,N-dimethylpropanamideHCID 11208889Bis(4-fluorophenyl)(piperidin-4-yl)methanol

生成物 1

HCID 19992280HCID 19992280、化合物収率 100%

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide
触媒
HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 10.0 g (0.033 mole) of α,α-bis(4-fluorophenyl)-4-piperidinemethanol, 4.5 g (0.033 mole) of 3-chloro-N,N-dimethylpropanamide, 14.0 g (0.132 mole) of anhydrous sodium carbonate and 0.3 g (0.002 mole) of potassium iodide in 100 ml of N,N-dimethylformamide was heated on a steam bath for 16 h. The mixture was poured into 2 L of water and extracted three times with 500 ml portions of ethyl acetate. The ethyl acetate fractions were combined, washed with water and brine, dried (MgSO4) and concentrated under reduced pressure to give a glass. Upon trituration with petroleum ether (30°-60° C.) the glass solidified to yield 13.2 g (100%) of a yellow solid. A portion of this solid was recrystallized from ethyl ether to give the title compound as a white solid, mp 134°-135° C.

後処理

  1. temperaturewas heated on a steam bath for 16 h
  2. extractionextracted three times with 500 ml portions of ethyl acetate
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure
  6. customto give a glass

出典と根拠

ORDレコード
ord-4c0a2f555d09421e99c9f7174d63de9d
出典データセット
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05057524

反応ノート

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