Methyl iodide → HCID 67653887, 화합물

HRID 2393339노트

반응식

HRID 2393339 반응식
[CH3:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([CH2:9][C:10]([O:12][CH3:13])=[O:11])=[C:4]([O:14][C:15]2[CH:16]=[N:17][N:18]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[CH3:26])[CH:19]=2)[N:3]=1.[H-].[Na+].C(CNC[CH:34]=[O:35])=O.[CH3:36]I>CN(C)C=O.COCCOC>[CH3:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([C:9](=[CH:36][O:35][CH3:34])[C:10]([O:12][CH3:13])=[O:11])=[C:4]([O:14][C:15]2[CH:16]=[N:17][N:18]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[CH3:26])[CH:19]=2)[N:3]=1

참가 물질

7

반응물 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 18975607HCID 18975607, 화합물HCID 202686642,2'-Azanediyldiacetaldehyde

생성물 1

HCID 67653887HCID 67653887, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
45 °C

실험 절차

The intermediate methyl 2-[2,4-dimethyl-6-(1-(2-methylphenyl)-1H-pyrazol-4-yloxy)-pyrimidin-5-yl]-acetate (6.0 g, 17 mmol), sodium hydride (0.9 g, 37 mmol) and N,N-diformylmethylamine (6 ml) in a mixture of dimethylformamide (20 ml) and 1,2-dimethoxyethane (20 ml) is stirred at 45° C. for 3 hours. Methyliodide (4.2 g, 30 mmol) is added at room temperature and stirring is continued for additional 16 hours. Dilution with ether, washing with brine, drying and chromatography on silicagel (eluant ethyl acetate/hexane 3:7) gives methyl 2-[2,4-dimethyl-6-(1-(2-methylphenyl)-1H-pyrazole-4-yloxy)-pyrimidin-5-yl]-3-methoxyacrylate as a colorless oil.

후처리

  1. stirringstirring
  2. waitis continued for additional 16 hours
  3. washDilution with ether, washing with brine
  4. customdrying

출처 및 근거

ORD 기록
ord-4a4730f52f544326813c7b8d75189987
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05807863

반응 노트

불러오는 중…