Water → 1-Ethyl-3-(2-methoxy-4-nitrophenyl)pyridin-2(1H)-one

HRID 218522ノート

反応式

HRID 218522 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=1[C:12]1[C:13](=[O:18])[NH:14][CH:15]=[CH:16][CH:17]=1.C(=O)([O-])[O-].[K+].[K+].I[CH2:26][CH3:27].O>CN(C=O)C>[CH2:26]([N:14]1[CH:15]=[CH:16][CH:17]=[C:12]([C:4]2[CH:5]=[CH:6][C:7]([N+:9]([O-:11])=[O:10])=[CH:8][C:3]=2[O:2][CH3:1])[C:13]1=[O:18])[CH3:27]

参加物

6

反応物 4

HCID 962WaterHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 595867673-(2-Methoxy-4-nitrophenyl)pyridin-2(1H)-one

生成物 1

HCID 595867171-Ethyl-3-(2-methoxy-4-nitrophenyl)pyridin-2(1H)-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

350 mg (1.42 mmol) of the product from example 55A are suspended in 3.5 ml of DMF. To this are added 393 mg (2.84 mmol) of potassium carbonate and 266 mg (1.71 mmol) of iodoethane, and the mixture is left to stir at RT for 3 h. Then it is admixed with water and extracted with dichloromethane. The organic solution is dried over sodium sulfate, concentrated and purified by preparative HPLC. This affords 224 mg (57% of theory) of the title compound.

後処理

  1. waitthe mixture is left
  2. extractionextracted with dichloromethane
  3. dry with materialThe organic solution is dried over sodium sulfate
  4. concentrationconcentrated
  5. custompurified by preparative HPLC

出典と根拠

ORDレコード
ord-22deb0e9c8cb406cbc008ac388982d1f
出典データセット
uspto-grants-2012_06
特許番号
US08198267B2

反応ノート

読み込み中…