Methyl iodide → HCID 19817746、化合物

HRID 1087181ノート

反応式

HRID 1087181 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 19817746HCID 19817746、化合物収率 84.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ad068f835b634fec9e7e354cc6fb894d
出典データセット
uspto-grants-1991_07
特許番号
US05034417

反応ノート

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