1,2-dibenzoyl-5-phenyl-1H-1,2,5-triazepine → 1,2-Dibenzoylhexahydro-1H-1,2,5-triazepine

HRID 2292276ノート

反応式

HRID 2292276 の反応式
[C:1]([N:9]1[CH:15]=[CH:14][N:13](C2C=CC=CC=2)[CH:12]=[CH:11][N:10]1[C:22](=[O:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>[Pd].O1CCOCC1>[C:1]([N:9]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11][N:10]1[C:22](=[O:29])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 1

HCID 212772361,2-dibenzoyl-5-phenyl-1H-1,2,5-triazepine

生成物 1

HCID 143909121,2-Dibenzoylhexahydro-1H-1,2,5-triazepine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 1,2-dibenzoyl-5-phenyl-1H-1,2,5-triazepine (25.0 g), dioxane (500 ml), N-hydrochloric acid (250 ml) and 10% Palladium on carbon (1.3 g) was hydrogenated in a Parr apparatus at 16 p.s.i. pressure for 191/2 hours. The catalyst was removed by filtration and washed with water. The filtrate and washings were evaporated to a solid hydrochloride salt which was dried under oil pump vacuum; wt. 22.4 g. The material was assayed by HPLC and shown to be 91% pure. Material prepared in this way was used directly in further syntheses, e.g., in example 8.

後処理

  1. custom2 hours
  2. customThe catalyst was removed by filtration
  3. washwashed with water
  4. customThe filtrate and washings were evaporated to a solid hydrochloride salt which
  5. customwas dried under oil pump vacuum
  6. customMaterial prepared in this way

出典と根拠

ORDレコード
ord-785ff56f60234e48a3669a962818a9f0
出典データセット
uspto-grants-1989_01
特許番号
US04801706

反応ノート

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