Dimethylformamide → HCID 178518278、化合物

HRID 2236687ノート

反応式

HRID 2236687 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[NH:7][C:6](=[O:13])/[C:5]/2=[CH:14]/OC.Cl.[NH2:18][CH2:19][C:20]1[CH:25]=[CH:24][NH:23][C:22](=[O:26])[CH:21]=1.CN(C)C=O.C(N(CC)CC)C>O1CCCC1.O>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[NH:7][C:6](=[O:13])/[C:5]/2=[CH:14]\[NH:18][CH2:19][C:20]1[CH:25]=[CH:24][NH:23][C:22](=[O:26])[CH:21]=1

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 574158824-(Aminomethyl)pyridin-2(1H)-one--hydrogen chloride (1/1)HCID 68692760(E)-6-bromo-4-(methoxymethylene)isoquinoline-1,3(2H,4H)-dione

生成物 1

HCID 178518278HCID 178518278、化合物収率 54%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

(4E)-6-bromo-4-(methoxymethylene)isoquinoline-1,3(2H,4H)-dione (0.26 g, 0.94 mmol) and 4-aminomethyl-1H-pyridin-2-one hydrochloride (0.15 g, 0.94 mmol) were coupled in tetrahydrofuran (5 mL) and N,N-dimethylformamide (3 mL) with triethylamine (0.28 g) at room temperature overnight. After the addition of water, the solid material is collected by Buchner filtration, washed with diethyl ether, water, and methanol, and dried under vacuum to give (4Z)-6-bromo-4-({[(2-oxo-1,2-dihydropyridin-4-yl)methyl]amino}methylene)isoquinoline-1,3(2H,4H)-dione (0.19 g, 54%) as a gray powder.

後処理

  1. customat room temperature
  2. customovernight
  3. filtrationthe solid material is collected by Buchner filtration
  4. washwashed with diethyl ether, water, and methanol
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-8d6e454cc0a048a9adc2c189dafbf054
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

反応ノート

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