Methyl iodide → HCID 67715083, 화합물

HRID 1682531노트

반응식

HRID 1682531 반응식
[CH3:1][C:2]1[N:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=2)[C:5]([CH2:19][C:20]([O:22][CH2:23]C)=[O:21])=[CH:4][N:3]=1.[H-].[Na+].CI.[CH:29]([O:31][CH3:32])=O>CCOCC>[CH3:1][C:2]1[N:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:16])([F:17])[F:18])[CH:10]=2)[C:5]([C:19](=[CH:29][O:31][CH3:32])[C:20]([O:22][CH3:23])=[O:21])=[CH:4][N:3]=1

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 7865Methyl formateHCID 24758Sodium hydrideHCID 19044668HCID 19044668, 화합물

생성물 1

HCID 67715083HCID 67715083, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Ethyl α-[2-methyl-4-(3-trifluoromethylphenoxy)-5-pyrimidinyl]-acetate (3 g, 8 mmol) are dissolved in methyl formate (10 ml) and added to a suspension of NaH (0.6 g, 80% in oil, 20 mmol) in 1,2-dimethoxyaethane at room temperature. After 16 hours methyl iodide (2.5 ml, 40 mmol) is added with cooling. After further 2 hours the reaction mixture is diluted with ether and washed with brine. Drying and chromatography on silicagel (eluant:hexane/ethyl acetate 1:1) gives the methyl α-[2-methyl-4-(3-trifluoromethylphenoxy)-5-pyrimidinyl]-β-methoxyacrylate compound as a crystalline solid, m.p. 100°-102° C.

후처리

  1. temperaturewith cooling
  2. washwashed with brine
  3. customDrying

출처 및 근거

ORD 기록
ord-1e64abfe3a99409a9e61f9ce153e6d36
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05635508

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