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Hydrochloric Acid → 5H-Pyrido(2,3-b)(1,5)benzodiazepin-5-one, 6,11-dihydro-11-methyl-

HRID 1898870
ノート
印刷プレビュー

反応式

HRID 1898870 の反応式
C([N:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[N:13]([CH3:20])[C:12]2[N:21]=[CH:22][CH:23]=[CH:24][C:11]=2[C:10]1=[O:25])(=O)C1C=CC=CC=1.Cl>C(O)C>[CH3:20][N:13]1[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[NH:9][C:10](=[O:25])[C:11]2[CH:24]=[CH:23][CH:22]=[N:21][C:12]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 23372616HCID 23372616、化合物

生成物 1

HCID 4532425H-Pyrido(2,3-b)(1,5)benzodiazepin-5-one, 6,11-dihydro-11-methyl-

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 9.4 g (0.0285 mol) of the product obtained in step b, 150 ml ethanol and 5 ml concentrated aqueous hydrochloric acid was refluxed for five hours while stirring. The clear yellowish solution that had been formed was set aside overnight. The resulting precipitate was collected by filtration and thoroughly washed with diluted aqueous ammonia. The product was dried overnight in a stream of nitrogen at room temperature and thereafter was recrystallized from n-propanol. The colorless product had a m.p. of 235°-237° C. and was identified as 6,11-dihydro-11-methyl-5H-pyrido-[2,3-b][1,5]benzodiazepin-5-one. The yield was 3.3 g (51% of theory).

後処理

  1. temperaturewas refluxed for five hours
  2. customThe clear yellowish solution that had been formed
  3. filtrationThe resulting precipitate was collected by filtration
  4. washthoroughly washed with diluted aqueous ammonia
  5. customThe product was dried overnight in a stream of nitrogen at room temperature
  6. customwas recrystallized from n-propanol

出典と根拠

ORDレコード
ord-4c31e871222f4032a54af35a52ccfe0d
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05571809

反応ノート

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