Methanol → HCID 12404883、化合物

HRID 1670862ノート

反応式

HRID 1670862 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 12404883HCID 12404883、化合物収率 86%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 3283Diethyl Ether溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-30fb12c0d2a2430eb4c08f3e2a95aad3
出典データセット
uspto-grants-2011_08
特許番号
US07994205B2

反応ノート

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