Sodium hydride → 5,11-dihydro-11-ethyl-2-methoxy-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one

HRID 53533ノート

反応式

HRID 53533 の反応式
[H-].[Na+].Br[C:4]1[C:9]([NH:10][C:11]([C:13]2[C:14]([NH:19][CH2:20][CH3:21])=[N:15][CH:16]=[CH:17][CH:18]=2)=[O:12])=[C:8]([CH3:22])[CH:7]=[C:6]([O:23][CH3:24])[N:5]=1>N1C=CC=CC=1.C(OCC)(=O)C>[CH2:20]([N:19]1[C:14]2[N:15]=[CH:16][CH:17]=[CH:18][C:13]=2[C:11](=[O:12])[NH:10][C:9]2[C:8]([CH3:22])=[CH:7][C:6]([O:23][CH3:24])=[N:5][C:4]1=2)[CH3:21]

参加物

5

反応物 2

HCID 24758Sodium hydrideHCID 19960032N-(2-Bromo-6-methoxy-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide

生成物 1

HCID 152212525,11-dihydro-11-ethyl-2-methoxy-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one収率 47.6%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Sodium hydride (0.14 g of a 50% dispersion in mineral oil) was added to a solution of N-(2-bromo-6-methoxy-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide (0.54 g) in pyridine (4 ml), and the resulting mixture was refluxed for 1.5 hours. The cooled mixture was diluted with ethyl acetate, washed with water, and the organic phase was dried (anhydrous magnesium sulfate) and concentrated. The residue was washed with diisopropyl ether and hot ethyl acetate, and then crystallized from ethanol to provide 0.2 g of 5,11-dihydro-11-ethyl-2-methoxy-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one, m.p. 249°-251° C.

後処理

  1. temperaturethe resulting mixture was refluxed for 1.5 hours
  2. washwashed with water
  3. dry with materialthe organic phase was dried (anhydrous magnesium sulfate)
  4. concentrationconcentrated
  5. washThe residue was washed with diisopropyl ether and hot ethyl acetate
  6. customcrystallized from ethanol

出典と根拠

ORDレコード
ord-dc6d4a62f6404ec5b1af4325c2f068cb
出典データセット
uspto-grants-1997_04
特許番号
US05620974

反応ノート

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