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Sodium hydride → HCID 20393023、化合物

HRID 1862983
ノート
印刷プレビュー

反応式

HRID 1862983 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH3:21])[C:5]2[C:11](=[O:12])[N:10]([CH3:13])[C:9]3[CH:14]=[C:15]([CH3:19])[C:16]([CH3:18])=[CH:17][C:8]=3[NH:7][C:6]=2[N:20]=1.[H-].[Na+].[CH2:24]([N:26]([CH2:31][CH3:32])[CH2:27][CH2:28][CH2:29]Cl)[CH3:25]>CN(C)C=O>[CH2:24]([N:26]([CH2:31][CH3:32])[CH2:27][CH2:28][CH2:29][N:7]1[C:8]2[CH:17]=[C:16]([CH3:18])[C:15]([CH3:19])=[CH:14][C:9]=2[N:10]([CH3:13])[C:11](=[O:12])[C:5]2[C:4]([CH3:21])=[CH:3][C:2]([CH3:1])=[N:20][C:6]1=2)[CH3:25]
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 23372624HCID 23372624、化合物

生成物 1

HCID 20393023HCID 20393023、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
50 °C

実験手順

A mixture consisting of 1.8 mg of 6,11-dihydro-2,4,6,8,9-pentamethyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one, 30 ml of dimethyl formamide and 0.34 gm of 50% sodium hydride in mineral oil was stirred in a nitrogen atmosphere at 50° C. for 30 minutes. Then, a solution of 1.5 gm of 3-diethylaminopropyl chloride in 15 ml of dimethyl formamide was added dropwise at room temperature, and the mixture was heated on an oil bath at 120° C. for 2 hours and then evaporated in vacuo. The residue was admixed with dilute ammonia, and the mixture was repeatedly extracted with ether. The combined ether extracts were dried with sodium sulfate, the ether was distilled off, and the residue was recrystallized from petroleum ether (m.p. 100°-140° C.), yielding 53% of theory of the compound named in the heading, which had a melting point of 104°-106° C.

後処理

  1. temperaturethe mixture was heated on an oil bath at 120° C. for 2 hours
  2. customevaporated in vacuo
  3. extractionthe mixture was repeatedly extracted with ether
  4. dry with materialThe combined ether extracts were dried with sodium sulfate
  5. distillationthe ether was distilled off
  6. customthe residue was recrystallized from petroleum ether (m.p. 100°-140° C.)
  7. customyielding 53% of theory of the compound

出典と根拠

ORDレコード
ord-946780e0377a43a4af75cee4ce5ad33b
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

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