Ethyl (E)-3-(4-oxo-7-trifluoromethyl-4,5-dihydropyrrolo[1,2-a]-quinoxalin-1-yl)acrylate → Ethyl 3-(4-oxo-7-trifluoromethyl-4,5-dihydropyrrolo[1,2-a]-quinoxalin-1-yl)propanoate

HRID 72749

반응식

HRID 72749 반응식
[O:1]=[C:2]1[NH:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:12]([F:15])([F:14])[F:13])[CH:9]=2)[N:4]2[C:16](/[CH:19]=[CH:20]/[C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:17][CH:18]=[C:3]12>[C].[Pd].C(O)(=O)C>[O:1]=[C:2]1[NH:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:12]([F:14])([F:13])[F:15])[CH:9]=2)[N:4]2[C:16]([CH2:19][CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:17][CH:18]=[C:3]12

참가 물질

4

반응물 1

HCID 59198853Ethyl (E)-3-(4-oxo-7-trifluoromethyl-4,5-dihydropyrrolo[1,2-a]-quinoxalin-1-yl)acrylate

생성물 1

HCID 59198598Ethyl 3-(4-oxo-7-trifluoromethyl-4,5-dihydropyrrolo[1,2-a]-quinoxalin-1-yl)propanoate

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 176Acetic Acid용매

실험 절차

Ethyl (E)-3-(4-oxo-7-trifluoromethyl-4,5-dihydropyrrolo[1,2-a]-quinoxalin-1-yl)acrylate as synthesized in Example 188, 182 mg, 5% palladium carbon 80 mg and acetic acid 6 mL were mixed and stirred under hydrogen atmosphere at room temperature for 16 hours. Filtering the reaction liquid through Celite, 50 mL of water was added to the filtrate and the precipitated crystals were recovered by filtration. The crystals were washed successively with water and diethyl ether, and dried in flowing air under heating to provide 120 mg of the title compound.

후처리

  1. additionwere mixed
  2. filtrationFiltering
  3. customthe reaction liquid through Celite, 50 mL of water
  4. additionwas added to the filtrate
  5. filtrationthe precipitated crystals were recovered by filtration
  6. washThe crystals were washed successively with water and diethyl ether
  7. customdried
  8. temperatureunder heating

출처 및 근거

ORD 기록
ord-0ae8295e5ed6406c98edfd56fb2bc7a9
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829000B2

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