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

HRID 1087183노트

반응식

HRID 1087183 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
200 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-712b1397105c49dfaec0dc1971e7beb1
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05034417

반응 노트

불러오는 중…