Triethylamine → HCID 86741629、化合物

HRID 653120ノート

反応式

HRID 653120 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH:12]1[CH2:14][CH2:13]1)[C:7](=[C:15]=[O:16])[CH2:6][C:5]2=[O:17].CO[CH:20](OC)[N:21]([CH3:23])[CH3:22].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]([CH:12]1[CH2:13][CH2:14]1)[C:7](=[C:15]=[O:16])[C:6](=[CH:20][N:21]([CH3:23])[CH3:22])[C:5]2=[O:17]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 78373Dimethylformamide dimethyl acetalHCID 867416286-Chloro-1-cycloprop yl-carbonyl-4-oxo-1,2,3,4-tetrahydroquinoline

生成物 1

HCID 86741629HCID 86741629、化合物収率 99.6%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 6-chloro-1-cyclopropyl-carbonyl-4-oxo-1,2,3,4-tetrahydroquinoline (1.996 g), N,N-dimethylformamide dimethyl acetal (3.808 g), and triethylamine (1.212 g) in benzene (16 ml) was refluxed with stirring for 30 minutes and then about three-fourths of the solvent was distilled slowly at atmospheric pressure over a period of approximately 30 minutes. To the residue was added benzene (16 ml) and the solvent was distilled again. The residue was dissolved in ethyl acetate, treated with activated charcoal, and evaporated in vacuo. The residual solid was washed with diethyl ether to give 6-chloro-1-cyclopropyl-carbonyl-3-dimethylaminomethylene-4-oxo-1,2,3,4-tetrahydroquinoline (2.43 g).

後処理

  1. distillationabout three-fourths of the solvent was distilled slowly at atmospheric pressure over a period of approximately 30 minutes
  2. additionTo the residue was added benzene (16 ml)
  3. distillationthe solvent was distilled again
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. additiontreated with activated charcoal
  6. customevaporated in vacuo
  7. washThe residual solid was washed with diethyl ether

出典と根拠

ORDレコード
ord-66dc1ba6056d41d4bf207fab094ad123
出典データセット
uspto-grants-1987_06
特許番号
US04675324

反応ノート

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