2-[(2-chloro-1-oxo-propyl)-amino]-beta-oxo-N-(2-pyridinyl)-3-trifluoromethyl-benzene-propanamide → HCID 178434920、化合物

HRID 1153799ノート

反応式

HRID 1153799 の反応式
Cl[CH:2]([CH3:28])[C:3]([NH:5][C:6]1[C:11]([C:12]([F:15])([F:14])[F:13])=[CH:10][CH:9]=[CH:8][C:7]=1[C:16](=[O:27])[CH2:17][C:18]([NH:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=1)=[O:19])=O>CN(C)C1C=CN=CC=1.O1CCCC1>[CH3:28][CH:2]1[C:3]2=[N:5][C:6]3[C:11]([C:12]([F:14])([F:15])[F:13])=[CH:10][CH:9]=[CH:8][C:7]=3[C:16]([OH:27])=[C:17]2[C:18](=[N:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=2)[O:19]1

参加物

4

反応物 1

HCID 134231002-[(2-chloro-1-oxo-propyl)-amino]-beta-oxo-N-(2-pyridinyl)-3-trifluoromethyl-benzene-propanamide

生成物 1

HCID 178434920HCID 178434920、化合物収率 115.2%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 8028Tetrahydrofuran溶媒

実験手順

1.60 g of 4-dimethylamino-pyridine were added to a suspension of 4.5 g of the product of Step A in 90 ml of tetrahydrofuran and the mixture was refluxed for four hours and was evaporated to dryness under reduced pressure. The residue was added to 90 ml of water and the mixture was stirred for 30 minutes and was vacuum filtered. The product was washed with water and dried under reduced pressure at 70° C. to obtain 4.50 g of 1,3-dihydro-3-methyl-1-[(2-pyridinyl)-imino]-5-trifluoromethyl-furo[3,4-b]quinoline-9-ol which was crystallized from absolute ethanol.

後処理

  1. temperaturethe mixture was refluxed for four hours
  2. customwas evaporated to dryness under reduced pressure
  3. additionThe residue was added to 90 ml of water
  4. filtrationfiltered
  5. washThe product was washed with water
  6. customdried under reduced pressure at 70° C.

出典と根拠

ORDレコード
ord-861f1f95e7444c59824576c41a54c274
出典データセット
uspto-grants-1984_12
特許番号
US04486438

反応ノート

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