Methyl iodide → HCID 54334135, 화합물

HRID 1885247노트

반응식

HRID 1885247 반응식
IC.[CH3:3][C:4]([C:7]1[CH:8]=[C:9]([CH:18]=[C:19]2[N:23]([CH3:24])[C:22](=[S:25])[NH:21][C:20]2=[O:26])[CH:10]=[C:11]([C:14]([CH3:17])([CH3:16])[CH3:15])[C:12]=1[OH:13])([CH3:6])[CH3:5].[CH:27](N(C(C)C)CC)(C)C>C(O)C.O>[CH3:6][C:4]([C:7]1[CH:8]=[C:9]([CH:18]=[C:19]2[N:23]([CH3:24])[C:22]([S:25][CH3:27])=[N:21][C:20]2=[O:26])[CH:10]=[C:11]([C:14]([CH3:15])([CH3:16])[CH3:17])[C:12]=1[OH:13])([CH3:3])[CH3:5]

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 81531DiisopropylethylamineHCID 53632063HCID 53632063, 화합물

생성물 1

HCID 54334135HCID 54334135, 화합물수율 69.3%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Iodomethane (1.2 mL, 19 mmols) is added to a stirred suspension of 5-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-1-methyl-2-thioxo-4-imidazolidinone (4.0 g, 12 mmols) and diisopropylethylamine (2.4 mL, 14 mmols) in ethanol (50 ml) and the mixture is stirred under an inert atmosphere at room temperature. After 18 hours the mixture is stirred in water (300 mL) for an hour and the product is filtered off, washed three times with water, and dried. Recrystallization from ethyl acetate gave the pure 5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-1,5-dihydro-1-methyl-2-(methylthio)-4H-imidazol-4-one (3.0 g), mp 177°-179° C., retaining 0.25 equivalents of solvent of crystallization.

후처리

  1. filtrationthe product is filtered off
  2. washwashed three times with water
  3. customdried
  4. customRecrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-3c49ebac8cad48caac2f36a0eeffe9d4
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05143928

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