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Sodium hydride → 6,11-Dihydro-2,6-dimethyl-11-(3-dimethylamino-propyl)-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one

HRID 1862976
ノート
印刷プレビュー

反応式

HRID 1862976 の反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[C:11](=[O:12])[N:10]([CH3:13])[C:9]3[CH:14]=[CH:15][CH:16]=[CH:17][C:8]=3[NH:7][C:6]=2[N:18]=1.[H-].[Na+].[CH2:21]([N:23]([CH2:28]C)[CH2:24][CH2:25][CH2:26]Cl)C>CN(C)C=O>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[C:11](=[O:12])[N:10]([CH3:13])[C:9]3[CH:14]=[CH:15][CH:16]=[CH:17][C:8]=3[N:7]([CH2:26][CH2:25][CH2:24][N:23]([CH3:28])[CH3:21])[C:6]=2[N:18]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 669183-Chloropropyl(diethyl)amineHCID 203930286,11-Dihydro-2,6-dimethyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one

生成物 1

HCID 203930256,11-Dihydro-2,6-dimethyl-11-(3-dimethylamino-propyl)-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
120 °C

実験手順

A mixture consisting of 7.2 gm of 6,11-dihydro-2,6-dimethyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one, 70 ml of dimethyl formamide and 1.9 gm of 50% sodium hydride in mineral oil was stirred at 30°-50° C. in a nitrogen atmosphere for 30 minutes. Then, a solution of 6.1 gm of 3-diethylamino-propyl chloride in 30 ml of dimethyl formamide was added dropwise, and the mixture was heated on an oil bath at 120° C. for 3 hours and then evaporated in vacuo. The residue was mixed with an aqueous potassium carbonate solution, and the mixture was extracted with ether. The ethereal phase was dried with sodium sulfate and evaporated, and the residue was recrystallized from petroleum ether (b.p. 100°-140° C.), yielding 76% of theory of the compound named in the heading, which had a melting point of 130°-131° C.

後処理

  1. customevaporated in vacuo
  2. additionThe residue was mixed with an aqueous potassium carbonate solution
  3. extractionthe mixture was extracted with ether
  4. dry with materialThe ethereal phase was dried with sodium sulfate
  5. customevaporated
  6. customthe residue was recrystallized from petroleum ether (b.p. 100°-140° C.)
  7. customyielding 76% of theory of the compound

出典と根拠

ORDレコード
ord-fbe1de0b0dea4a48925d96834c981e64
出典データセット
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04167570

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート