Methyl iodide → HCID 21833808, 화합물

HRID 1741090노트

반응식

HRID 1741090 반응식
[O:1]1[CH2:5][CH2:4][N:3]=[C:2]1[C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:17]=[CH:16][C:15]([C:18]([OH:20])=[O:19])=[CH:14][CH:13]=2)=[C:8]([CH3:21])[CH:7]=1.[H-].[Na+].I[CH3:25]>CN(C=O)C.C(OCC)(=O)C>[O:1]1[CH2:5][CH2:4][N:3]=[C:2]1[C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:13]=[CH:14][C:15]([C:18]([O:20][CH3:25])=[O:19])=[CH:16][CH:17]=2)=[C:8]([CH3:21])[CH:7]=1

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 218338564'-(4,5-Dihydrooxazol-2-yl)-2'-methylbiphenyl-4-carboxylic acid

생성물 1

HCID 21833808HCID 21833808, 화합물수율 15.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

4'-(4,5-Dihydrooxazol-2-yl)-2'-methylbiphenyl-4-carboxylic acid (D113) (0.92 g, 3.3 mmol) was stirred under Ar in dry DMF (20 ml), and sodium hydride (80% in mineral oil, 0.15 g, 5.0 mmol) was added. This mixture was stirred for 30 min, and then treated with iodomethane (0.22 ml, 3.5 mmol). After a further 15 min, the mixture was diluted with ethyl acetate (200 ml), washed with water and brine, dried (Na2SO4) and evaporated. The crude product was purified by chromatography on silica gel, eluting with 0-2% methanol/dichloromethane. This gave the title compound (0.15 g, 15%) as a white solid.

후처리

  1. waitAfter a further 15 min
  2. washwashed with water and brine
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customThe crude product was purified by chromatography on silica gel
  6. washeluting with 0-2% methanol/dichloromethane

출처 및 근거

ORD 기록
ord-96235dbdae7b40bab0facbd1a9a196f6
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05972951

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