Water → 2-Methyl-2-nitro-1-(methoxymethoxy)propane

HRID 636736노트

반응식

HRID 636736 반응식
[CH3:1][C:2]([N+:6]([O-:8])=[O:7])([CH3:5])[CH2:3][OH:4].[Li+].[Br-].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.O.[CH3:24][O:25][CH2:26]OC>>[CH3:1][C:2]([N+:6]([O-:8])=[O:7])([CH3:5])[CH2:3][O:4][CH2:24][O:25][CH3:26]

참가 물질

6

반응물 5

HCID 962WaterHCID 64422-Methyl-2-nitro-1-propanolHCID 8020DimethoxymethaneHCID 82050Lithium BromideHCID 521998p-Toluenesulfonic acid monohydrate

생성물 1

HCID 212556992-Methyl-2-nitro-1-(methoxymethoxy)propane수율 76%

실험 절차

To a solution of 2-methyl-2-nitro-1-propanol (366.8 mg, 3.08 mmol) and LiBr (60.8 mg, 0.700 mmol) in dimethoxymethane (5 ml) was added p-toluenesulfonic acid hydrate (56.3 mg, 0.296 mmol) and stirred for 24 hours. The mixture was added to water and extracted three times with ethyl acetate and dried over MgSO4. The mixture was concentrated and purified by silica gel chromatography (hexane/ether=4/1) to give the title compound (382.7 mg; 76%).

후처리

  1. extractionextracted three times with ethyl acetate
  2. dry with materialdried over MgSO4
  3. concentrationThe mixture was concentrated
  4. custompurified by silica gel chromatography (hexane/ether=4/1)

출처 및 근거

ORD 기록
ord-65625b631df84f3c80df010961eff1d7
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194461B1

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