Chloroacetyl chloride → N-(2-Anilinophenyl)-2-chloroacetamide

HRID 1709632

반응식

HRID 1709632 반응식
[C:1]1([NH:7][C:8]2[C:9]([NH2:14])=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[Cl:22][CH2:23][C:24](Cl)=[O:25]>C(Cl)(Cl)Cl.O>[Cl:22][CH2:23][C:24]([NH:14][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=1[NH:7][C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)=[O:25]

참가 물질

6

반응물 3

HCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 68297N-Phenyl-o-phenylenediamine

생성물 1

HCID 14819969N-(2-Anilinophenyl)-2-chloroacetamide수율 106%

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

In 100 ml of chloroform, 10.4 g of N-phenyl-1,2-benzenediamine and 12.1 g of triethylamine were dissolved, and the mixture was cooled to -5° C. to 0° C., and then 13.6 g of chloroacetyl chloride was added dropwise thereto, holding the temperature of the mixture at not higher than 20° C. The reaction nearly went to completion when the addition was finished. After stirring for further 30 minutes, the reaction mixture was diluted with 50 ml of water. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate and then the solvent is evaporated under reduced pressure. The resulting solid was recrystallized from ethanol to give 15.6 g of crystals having a melting point of 112° C. to 113° C. Yield: 60.0%.

후처리

  1. temperaturethe mixture was cooled to -5° C. to 0° C.
  2. customhigher than 20° C
  3. customThe reaction
  4. additionthe addition
  5. customThe organic layer was separated
  6. washwashed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customthe solvent is evaporated under reduced pressure
  9. customThe resulting solid was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-37906dc48d31413d9bf4a7aee1b72f6b
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04950667

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