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Acetic Acid → HCID 135705340, 화합물

HRID 1112260
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HRID 1112260 반응식
[NH2:1][C:2]1[C:11]([C:12]([NH2:14])=[O:13])=[C:10]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[C:21](OCC)(=O)[C:22]([O:24][CH2:25][CH3:26])=[O:23].C(O)(=O)C>CCOCC>[C:15]1([C:10]2[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=[C:2]3[N:1]=[C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[NH:14][C:12](=[O:13])[C:11]=23)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 7268Diethyl OxalateHCID 218217142-Amino-4-phenyl-3-quinolinecarboxamide

생성물 1

HCID 135705340HCID 135705340, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 2-amino-4-phenylquinoline-3-carboxamide (263 mg., 1.0 millimole), diethyl oxalate (5 ml.) acetic acid (5 ml.) is heated to reflux overnight. It is then cooled, diluted with ether (50 ml.) and the brown solid which forms filtered off. The filtrate is evaporated in vacuo and the oily residue triturated with saturated aqueous sodium bicarbonate solution. The resulting solid (110 mg.) is recovered by filtration and recrystallized from hot ethyl acetate (8 ml.). A small amount of insoluble material is filtered off from the hot solution. Upon cooling, the title product separates as crystals (25 mg.). M.P. = 255° C. (dec.).

후처리

  1. temperatureis heated
  2. temperatureto reflux overnight
  3. temperatureIt is then cooled
  4. filtrationthe brown solid which forms filtered off
  5. customThe filtrate is evaporated in vacuo
  6. customthe oily residue triturated with saturated aqueous sodium bicarbonate solution
  7. filtrationThe resulting solid (110 mg.) is recovered by filtration
  8. customrecrystallized from hot ethyl acetate (8 ml.)
  9. filtrationA small amount of insoluble material is filtered off from the hot solution
  10. temperatureUpon cooling

출처 및 근거

ORD 기록
ord-4704a3b3da2b46f598169897cd852c4c
출처 데이터셋
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04120962

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