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Water → 1-Benzhydryl-3-cyclopropyl-3-methoxyazetidine

HRID 1187750
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HRID 1187750 반응식
[CH:1]([N:14]1[CH2:17][C:16]([CH:19]2[CH2:21][CH2:20]2)([OH:18])[CH2:15]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH3:24]I.O>CN(C)C=O>[CH:1]([N:14]1[CH2:17][C:16]([CH:19]2[CH2:20][CH2:21]2)([O:18][CH3:24])[CH2:15]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 532567381-Benzhydryl-3-cyclopropylazetidin-3-ol

생성물 1

HCID 670081921-Benzhydryl-3-cyclopropyl-3-methoxyazetidine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

334 mg of 1-benzhydryl-3-cyclopropylazetidin-3-ol was dissolved in dimethylformamide, and 72 mg of 60% sodium hydride was added thereto, and the mixture was stirred at room temperature for 30 minutes. 112 μl of methyl iodide was added thereto, and the mixture was further stirred at room temperature for 2 hours. To the reaction solution was added water and the mixture was subjected to extraction with diethyl ether, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and then the obtained residue was purified by silica gel column chromatography to obtain 280 mg of the objective compound.

후처리

  1. stirringthe mixture was further stirred at room temperature for 2 hours
  2. extractionthe mixture was subjected to extraction with diethyl ether
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-ae490cf6bace43a49f8f773f2e4f5483
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08673891B2

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