Pentafluoroaniline → 4-(Pentafluorophenyl)-1-carbethoxysemicarbazide

HRID 1902894

반응식

HRID 1902894 반응식
[F:1][C:2]1[C:7]([NH2:8])=[C:6]([F:9])[C:5]([F:10])=[C:4]([F:11])[C:3]=1[F:12].[C:13]([NH:18][NH:19][C:20](Cl)=[O:21])([O:15][CH2:16][CH3:17])=[O:14]>C1(C)C=CC=CC=1>[F:1][C:2]1[C:7]([NH:8][C:20](=[O:21])[NH:19][NH:18][C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:6]([F:9])[C:5]([F:10])=[C:4]([F:11])[C:3]=1[F:12]

참가 물질

4

반응물 2

HCID 13040PentafluoroanilineHCID 84905Ethyl 3-(chloroformyl)carbazate

생성물 1

HCID 129043764-(Pentafluorophenyl)-1-carbethoxysemicarbazide

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Pentafluoroaniline (17 g, 0.106 mol) is dissolved in 300 ml of toluene with heating. The 2-carbethoxyhydrazinecarbonyl chloride, 19.4 g (0.122 M) is added to the hot solution. The mixture is refluxed until a white solid precipitates. The solid is filtered to give 24.8 g. The product is crystallized by dissolving in ethyl acetate/toluene (1/2 by vol) and evaporating until crystals appear, mp 180°-182°.

후처리

  1. temperaturewith heating
  2. temperatureThe mixture is refluxed until a white solid
  3. customprecipitates
  4. filtrationThe solid is filtered
  5. customto give 24.8 g
  6. customThe product is crystallized
  7. dissolutionby dissolving in ethyl acetate/toluene (1/2 by vol)
  8. customevaporating until crystals

출처 및 근거

ORD 기록
ord-b334485fa2c94ba2950c7cabf8f1c405
출처 데이터셋
uspto-grants-1982_12
특허 번호
US04366320

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