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

HRID 218522노트

반응식

HRID 218522 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-22deb0e9c8cb406cbc008ac388982d1f
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198267B2

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