Methanol → HCID 12404883, 화합물

HRID 1670862

반응식

HRID 1670862 반응식
[N+:1]([CH:4]([CH3:13])[CH:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[OH:6])([O-:3])=[O:2].[C:14](OC(=O)C)(=[O:16])[CH3:15].CO>C(OCC)C.CN(C)C1C=CN=CC=1>[C:14]([O:6][CH:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH:4]([N+:1]([O-:3])=[O:2])[CH3:13])(=[O:16])[CH3:15]

참가 물질

6

반응물 3

HCID 887MethanolHCID 7918Acetic AnhydrideHCID 2261182-Nitro-1-phenyl-1-propanol

생성물 1

HCID 12404883HCID 12404883, 화합물수율 86%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 3283Diethyl Ether용매

실험 절차

To a solution of 2-nitro-1-phenylpropan-1-ol (32 g) and acetic anhydride (22 mL) in diethyl ether (300 mL) was added 4-dimethylaminopyridine (0.61 g) under ice-cooling, and the mixture was stirred at room temperature for 1 hr. Methanol was added to the reaction mixture, and the mixture was further stirred for 30 min and concentrated under reduced pressure. Water was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution, water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give the title compound as a yellow oil (yield 34 g, 86%).

후처리

  1. temperaturecooling
  2. stirringthe mixture was further stirred for 30 min
  3. concentrationconcentrated under reduced pressure
  4. additionWater was added to the residue
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe extract was washed with saturated aqueous sodium hydrogen carbonate solution, water and saturated brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-30fb12c0d2a2430eb4c08f3e2a95aad3
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994205B2

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