Methyl iodide → HCID 19817746, 화합물

HRID 1087181노트

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HRID 1087181 반응식
[H-].[Na+].[F:3][C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[NH:11][C:12]1[CH:13]=[C:14]([C:21]2([CH3:26])[O:25][CH2:24][CH2:23][O:22]2)[CH:15]=[CH:16][C:17]=1[N+:18]([O-:20])=[O:19].[CH3:27]I>CN(C)C=O>[CH3:27][N:11]([C:12]1[CH:13]=[C:14]([C:21]2([CH3:26])[O:22][CH2:23][CH2:24][O:25]2)[CH:15]=[CH:16][C:17]=1[N+:18]([O-:20])=[O:19])[C:5]1[CH:6]=[CH:7][C:8]([F:10])=[CH:9][C:4]=1[F:3]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 103149282-[3-(2,4-Difluorophenylamino)-4-nitrophenyl]-2-methyl-1,3-dioxolane

생성물 1

HCID 19817746HCID 19817746, 화합물수율 84.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

Sodium hydride (60%; 0.14 g) was added portionwise to an ice-cooled solution of 2-[3-(2,4-difluorophenylamino)-4-nitrophenyl]-2-methyl-1,3-dioxolane (1 g) in N,N-dimethylformamide. To the resulting mixture as added methyl iodide (1.7 g). The mixture was stirred at 0° C. for 30 minutes, poured into ice-water (50 ml) and extracted with ethyl acetate. The extract was washed with water, dried and evaporated. The oily residue was purified by column chromatography on silica gel (30 g) eluting with toluene to give an oil of 2-{3-[N-methyl-N-(2,4-difluorophenyl)amino]-4-nitrophenyl}-2-methyl-1,3-dioxolane (0.88 g).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. customevaporated
  5. customThe oily residue was purified by column chromatography on silica gel (30 g)
  6. washeluting with toluene

출처 및 근거

ORD 기록
ord-ad068f835b634fec9e7e354cc6fb894d
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05034417

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