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Triethylamine → 6-Chloro-3-methylaminomethylene-4-oxo-1-propionyl-1,2,3,4-tetrahydroquinoline

HRID 35668
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반응식

HRID 35668 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]([C:12](=[O:15])[CH2:13][CH3:14])[CH2:7][CH2:6][C:5]2=[O:16].CO[CH:19](OC)[N:20](C)[CH3:21].C(N(CC)CC)C>C1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]([C:12](=[O:15])[CH2:13][CH3:14])[CH2:7][C:6](=[CH:19][NH:20][CH3:21])[C:5]2=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 78373Dimethylformamide dimethyl acetalHCID 145014226-Chloro-4-oxo-1-propionyl-1,2,3,4-tetrahydroquinoline

생성물 1

HCID 542284186-Chloro-3-methylaminomethylene-4-oxo-1-propionyl-1,2,3,4-tetrahydroquinoline수율 86.1%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A solution of 6-chloro-4-oxo-1-propionyl-1,2,3,4-tetrahydroquinoline (2 g), N,N-dimethylformamide dimethyl acetal (7.009 g), and triethylamine (0.87 g) in benzene (50 m) was refluxed with stirring for 1 hour and then about three-fourths of the solvent was distilled slowly at atmospheric pressure over a period ximately 1 hour. To the residue was added benzene (100 ml) and the solvent was distilled again. The resulting solid was collected by filtration, washed with diethyl ether, and dried to give 6-chloro-3-methylaminomethylene-4-oxo-1-propionyl-1,2,3,4-tetrahydroquinoline (2.02 g).

후처리

  1. distillationabout three-fourths of the solvent was distilled slowly at atmospheric pressure over a period ximately 1 hour
  2. additionTo the residue was added benzene (100 ml)
  3. distillationthe solvent was distilled again
  4. filtrationThe resulting solid was collected by filtration
  5. washwashed with diethyl ether
  6. customdried

출처 및 근거

ORD 기록
ord-a0798f33254e49d4856614cee3bd6850
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04767780

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