Methyl iodide → 5-Chloro-1-methylpyrazin-2(1H)-one

HRID 2045993노트

반응식

HRID 2045993 반응식
[Cl:1][C:2]1[N:3]=[CH:4][C:5]([OH:8])=[N:6][CH:7]=1.[C:9]([O-])([O-])=O.[K+].[K+].CI>CN(C=O)C>[Cl:1][C:2]1[N:3]=[CH:4][C:5](=[O:8])[N:6]([CH3:9])[CH:7]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178516772HCID 178516772, 화합물

생성물 1

HCID 584852805-Chloro-1-methylpyrazin-2(1H)-one수율 64%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5-chloro-pyrazin-2-ol (100 mg, 0.76 mmol) in DMF (3 mL) was added K2CO3 (211 mg, 1.53 mmol) and CH3I (0.25 ml, 4 mmol) at room temperature. The mixture was stirred overnight, quenched by H2O, and extracted with EtOAc. The organic phase was concentrated to give the crude product, which was purified by TLC to give 5-chloro-1-methyl-1H-pyrazin-2-one (70 mg, 64%). 1H NMR (CD3OD): δ3.52 (s, 3H), 7.78 (s, 1H), 7.87 (s, 1H).

후처리

  1. customquenched by H2O
  2. extractionextracted with EtOAc
  3. concentrationThe organic phase was concentrated
  4. customto give the crude product, which
  5. customwas purified by TLC

출처 및 근거

ORD 기록
ord-6c705502f0c04bddb05a3a25fe0af626
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08592410B2

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