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2-Methyl-2-nitro-1-propanol → 2-Methyl-2-nitro-1-benzyloxypropane

HRID 636745
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HRID 636745 반응식
[CH3:1][C:2]([N+:6]([O-:8])=[O:7])([CH3:5])[CH2:3][OH:4].[CH2:9](Br)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>CN(C=O)C>[CH3:1][C:2]([N+:6]([O-:8])=[O:7])([CH3:5])[CH2:3][O:4][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 64422-Methyl-2-nitro-1-propanolHCID 7498Benzyl Bromide

생성물 1

HCID 212556982-Methyl-2-nitro-1-benzyloxypropane수율 15.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a suspension of 2-methyl-2-nitro-1-propanol (2.3975 g, 20.13 mmol) and Ag2O (4.6385 g, 20.02 mmol) in DMF (25 ml) was added benzyl bromide (2.65ml, 22.28 mmol) and stirred for 48 hours. The mixture was filtered and the filtrate was added to 5% KHSO4 aqueous solution, extracted three times with ethyl acetate/hexane=1/1 and dried over MgSO4. The mixture was concentrated and purified by silica gel chromatography (toluene) to give the title compound (639.4 mg; 15%).

후처리

  1. filtrationThe mixture was filtered
  2. additionthe filtrate was added to 5% KHSO4 aqueous solution
  3. extractionextracted three times with ethyl acetate/hexane=1/1
  4. dry with materialdried over MgSO4
  5. concentrationThe mixture was concentrated
  6. custompurified by silica gel chromatography (toluene)

출처 및 근거

ORD 기록
ord-0c3531021adb42db8a83f78644452a53
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06194461B1

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