Iodoethane → N11-Ethyl-N5-methyl-5,11-dihydro-6H-dipyrido(3,2-b:2',3'-e)(1,4)diazepin-6-one

HRID 53512ノート

反応式

HRID 53512 の反応式
[H-].[Na+].[CH3:3][N:4]1[C:10](=[O:11])[C:9]2[CH:12]=[CH:13][CH:14]=[N:15][C:8]=2[NH:7][C:6]2[N:16]=[CH:17][CH:18]=[CH:19][C:5]1=2.[H][H].[CH2:22](I)[CH3:23]>CN(C)C=O.O>[CH2:22]([N:7]1[C:8]2[N:15]=[CH:14][CH:13]=[CH:12][C:9]=2[C:10](=[O:11])[N:4]([CH3:3])[C:5]2[CH:19]=[CH:18][CH:17]=[N:16][C:6]1=2)[CH3:23]

参加物

7

反応物 4

HCID 6340IodoethaneHCID 24758Sodium hydride2 回HCID 148738055,11-dihydro-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-oneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 453307N11-Ethyl-N5-methyl-5,11-dihydro-6H-dipyrido(3,2-b:2',3'-e)(1,4)diazepin-6-one収率 70.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

2.00 g of a 50% dispersion of sodium hydride in mineral oil was added to a solution of 5.75 g (0.025 mol) of 5,11-dihydro-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one in 100 ml of dimethylformamide. When the evolution of hydrogen ceased, the mixture was heated to 50° C. for 30 min. and then cooled to room temperature. Then, 7.80 g of ethyl iodide (neat) was added dropwise over 15 minutes, and the resulting mixture was allowed to stir overnight at room temperature. The excess sodium hydride was decomposed by the careful addition of ice, followed by water. The product was extracted with ether, dried (anhydrous sodium sulfate), and evaporated to yield 4.5 g (70% of theory) of 5,11-dihydro-11-ethyl-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one, m.p. 130°-132° C.

後処理

  1. temperaturecooled to room temperature
  2. extractionThe product was extracted with ether
  3. dry with materialdried (anhydrous sodium sulfate)
  4. customevaporated

出典と根拠

ORDレコード
ord-1ca77de4ad8446c98bcbca3bac2dd962
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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