Methyl iodide → 3-chloro-1-methyl-5-nitropyridin-2(1H)-one

HRID 873799노트

반응식

HRID 873799 반응식
[Cl:1][C:2]1[C:3]([OH:11])=[N:4][CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1.[C:12]([O-])([O-])=O.[K+].[K+].CI>CN(C=O)C>[Cl:1][C:2]1[C:3](=[O:11])[N:4]([CH3:12])[CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178526838HCID 178526838, 화합물

생성물 1

HCID 867031063-chloro-1-methyl-5-nitropyridin-2(1H)-one수율 96%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred suspension of 3-chloro-2-hydroxy-5-nitropyridine (10 g, 57.3 mmol) and K2CO3 (15.84 g, 115 mmol) in DMF (100 mL) under Ar was added MeI (5.37 mL, 86 mmol) at 0° C. The reaction mixture was stirred for 1 hr at rt, concentrated, diluted with water, and extracted with EtOAc. The combined organic layers were washed with water, dried over Na2SO4, and evaporated to afford the title product (10.38 g, 55.0 mmol, 96% yield) as a yellow solid. tR: 2.90 min (HPLC 1).

후처리

  1. concentrationconcentrated
  2. additiondiluted with water
  3. extractionextracted with EtOAc
  4. washThe combined organic layers were washed with water
  5. dry with materialdried over Na2SO4
  6. customevaporated

출처 및 근거

ORD 기록
ord-7df3e46ab469405eba3a757eddd74bb2
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975417B2

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