Piperazine → o-Methoxycarbonyl-alpha-(1-piperazinyl)acetanilide

HRID 1381184노트

반응식

HRID 1381184 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[CH2:8][C:9]([NH:11][C:12]1[CH:21]=[CH:20][CH:19]=[CH:18][C:13]=1[C:14]([O:16][CH3:17])=[O:15])=[O:10]>C(O)C>[CH3:17][O:16][C:14]([C:13]1[CH:18]=[CH:19][CH:20]=[CH:21][C:12]=1[NH:11][C:9](=[O:10])[CH2:8][N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)=[O:15]

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 295954Methyl 2-[(chloroacetyl)amino]benzoate

생성물 1

HCID 13117362o-Methoxycarbonyl-alpha-(1-piperazinyl)acetanilide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4.3 Grams of piperazine was added to 50 ml of ethanol, to this solution was added 2.3 g of methyl o-(α-chloroacetylamino)benzoate at a temperature of 40°-50° C. with stirring. The reaction mixture was stirred at the same temperature for 3 hours, then the reaction mixture was concentrated, to the obtained residue was added 20 ml of water, then saturated with sodium chloride, and extracted with chloroform. The chloroform layer was washed with a 10%-sodium hydroxide solution, then washed with a small amount of water and dried. After removal of the solvent by distillation, the residue obtained was purified by a silica gel column chromatography, and recrystallized from ether to obtain 2 g of o-methoxycarbonyl-α-(1-piperazinyl)-acetanilide in the form of colorless needle-like crystals. Melting point: 94°-96° C.

후처리

  1. stirringThe reaction mixture was stirred at the same temperature for 3 hours
  2. concentrationthe reaction mixture was concentrated, to the obtained residue
  3. additionwas added 20 ml of water
  4. extractionsaturated with sodium chloride, and extracted with chloroform
  5. washThe chloroform layer was washed with a 10%-sodium hydroxide solution
  6. washwashed with a small amount of water
  7. customdried
  8. customAfter removal of the solvent
  9. distillationby distillation
  10. customthe residue obtained
  11. customwas purified by a silica gel column chromatography
  12. customrecrystallized from ether

출처 및 근거

ORD 기록
ord-8194e563d1154bfb972dafdb7e017474
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04585774

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