2,4-Dichloroaniline → 2-[3-(2,4-Dichlorophenylamino)-4-nitrophenyl]-2-methyl-1,3-dioxolane

HRID 1087183ノート

反応式

HRID 1087183 の反応式
Cl[C:2]1[CH:3]=[C:4]([C:11]2([CH3:16])[O:15][CH2:14][CH2:13][O:12]2)[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].[Cl:17][C:18]1[CH:24]=[C:23]([Cl:25])[CH:22]=[CH:21][C:19]=1[NH2:20].C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C>[Cl:17][C:18]1[CH:24]=[C:23]([Cl:25])[CH:22]=[CH:21][C:19]=1[NH:20][C:2]1[CH:3]=[C:4]([C:11]2([CH3:16])[O:15][CH2:14][CH2:13][O:12]2)[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9]

参加物

5

反応物 3

HCID 111232,4-DichloroanilineHCID 11430Potassium CarbonateHCID 100374432-(3-Chloro-4-nitrophenyl)-2-methyl-1,3-dioxolane

生成物 1

HCID 198177092-[3-(2,4-Dichlorophenylamino)-4-nitrophenyl]-2-methyl-1,3-dioxolane収率 80%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
200 °C

実験手順

A mixture of 2-(3-chloro-4-nitrophenyl)-2-methyl-1,3-dioxolane (8 g), 2,4-dichloroaniline (10.6 g), cupric oxide (0.8 g) and potassium carbonate (5.4 g) was stirred for 3 hours at 200° C. Ethyl acetate (100 ml) was added to the mixture, stirred and filtered. The filtrate was washed with water, dried and evaporated to dryness. The oil (15.5 g) was purified by column chromatography on silica gel (150 g) eluting with toluene to give an oil of 2-[3-(2,4-dichlorophenylamino)-4-nitrophenyl]-2-methyl-1,3-dioxolane (9.7 g).

後処理

  1. stirringstirred
  2. filtrationfiltered
  3. washThe filtrate was washed with water
  4. customdried
  5. customevaporated to dryness
  6. customThe oil (15.5 g) was purified by column chromatography on silica gel (150 g)
  7. washeluting with toluene

出典と根拠

ORDレコード
ord-712b1397105c49dfaec0dc1971e7beb1
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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