Tris(hydroxymethyl)nitromethane → 1-benzyl-6-hydroxymethyl-4-methyl-6-nitrohexahydro-1H-1,4-diazepine

HRID 374112

反応式

HRID 374112 の反応式
[OH:1][CH2:2][C:3]([CH2:9]O)([CH2:7]O)[N+:4]([O-:6])=[O:5].C(=O)(O)[O-].[Na+].[CH2:16]([NH:23][CH2:24][CH2:25][NH:26][CH3:27])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O>[CH2:16]([N:23]1[CH2:9][C:3]([CH2:2][OH:1])([N+:4]([O-:6])=[O:5])[CH2:7][N:26]([CH3:27])[CH2:25][CH2:24]1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

5

反応物 3

HCID 31337Tris(hydroxymethyl)nitromethaneHCID 516892Sodium BicarbonateHCID 10920861N~1~-Benzyl-N~2~-methylethane-1,2-diamine

生成物 1

HCID 149386381-benzyl-6-hydroxymethyl-4-methyl-6-nitrohexahydro-1H-1,4-diazepine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

To a mixture of tris(hydroxymethyl)nitromethane (118.9 g), sodium bicarbonate (40 g) and water (1000 ml), N-benzyl-N'-methylethylenediamine (123 g) is added, and the reaction mixture is heated at about 50° C. for 2 hours. After cooling, the solution is extracted with dichloromethane, and the organic layer is washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The solvent is evaporated under reduced pressure to give 1-benzyl-6-hydroxymethyl-4-methyl-6-nitrohexahydro-1H-1,4-diazepine as an oil.

後処理

  1. additionis added
  2. temperatureAfter cooling
  3. extractionthe solution is extracted with dichloromethane
  4. washthe organic layer is washed with saturated aqueous sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent is evaporated under reduced pressure

出典と根拠

ORDレコード
ord-a9b2f3e1505e4ee9b870b600161f91c4
出典データセット
uspto-grants-1992_11
特許番号
US05166341

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