Sodium hydride → HCID 20306008、化合物

HRID 1732339ノート

反応式

HRID 1732339 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([OH:10])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[H-].[Na+].S(O[CH2:18][CH2:19][O:20][C:21]1[C:26]([O:27][CH3:28])=[CH:25][CH:24]=[CH:23][C:22]=1[O:29][CH3:30])(=O)(=O)C>>[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([O:10][CH2:18][CH2:19][O:20][C:21]2[C:26]([O:27][CH3:28])=[CH:25][CH:24]=[CH:23][C:22]=2[O:29][CH3:30])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

参加物

4

反応物 3

HCID 24758Sodium hydrideHCID 107492911-(4-Hydroxypiperidin-1-yl)ethan-1-oneHCID 20306015HCID 20306015、化合物

生成物 1

HCID 20306008HCID 20306008、化合物収率 61.8%

実験手順

N-Acetyl-4-hydroxypiperidine (4.3 g.) in D.M.F. (50 ml.) was added dropwise to a stirred suspension of sodium hydride (3.0 g., 50% dispersion in mineral oil) in D.M.F. (50 ml.) under an atmosphere of nitrogen. After stirring for 3 hours at room temperature 2-[2,6-dimethoxyphenoxy]ethyl mesylate (9.0 g.) in D.M.F. (50 ml.) was added dropwise and stirring continued for 20 hours at room temperature. The solvent was evaporated in vacuo, the residue taken up in water, extracted with chloroform (3×100 ml.), the organic layer dried (Na2SO4) and the solvent evaporated. Distillation gave N-acetyl-4-(2-[2,6-dimethoxyphenoxy]ethoxy)piperidine (6.0 g.), b.p. 200° C. @ 1 mm.

後処理

  1. addition(50 ml.) was added dropwise
  2. customThe solvent was evaporated in vacuo
  3. extractionextracted with chloroform (3×100 ml.)
  4. dry with materialthe organic layer dried (Na2SO4)
  5. customthe solvent evaporated
  6. distillationDistillation

出典と根拠

ORDレコード
ord-125bac00048e4b1fb7df492330a7f707
出典データセット
uspto-grants-1980_12
特許番号
US04237138

反応ノート

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