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

HRID 374112
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HRID 374112 반응식
[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
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참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a9b2f3e1505e4ee9b870b600161f91c4
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05166341

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