Sodium hydride → HCID 20306008, 화합물

HRID 1732339노트

반응식

HRID 1732339 반응식
[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]

참가 물질

4

반응물 3

HCID 24758Sodium hydrideHCID 107492911-(4-Hydroxypiperidin-1-yl)ethan-1-oneHCID 20306015HCID 20306015, 화합물

생성물 1

HCID 20306008HCID 20306008, 화합물수율 61.8%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-125bac00048e4b1fb7df492330a7f707
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04237138

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