Benzylamine → 3-nitryloxy-2,2-bis(nitryloxymethyl)propionic acid N-benzylamide

HRID 840192ノート

反応式

HRID 840192 の反応式
[N+:1]([O:4][CH2:5][C:6]([CH2:16][O:17][N+:18]([O-:20])=[O:19])([CH2:11][O:12][N+:13]([O-:15])=[O:14])[C:7](OC)=[O:8])([O-:3])=[O:2].[CH2:21]([NH2:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.[Cl-].[NH4+]>C(Cl)(Cl)Cl>[CH2:21]([NH:28][C:7](=[O:8])[C:6]([CH2:16][O:17][N+:18]([O-:20])=[O:19])([CH2:11][O:12][N+:13]([O-:15])=[O:14])[CH2:5][O:4][N+:1]([O-:3])=[O:2])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

参加物

5

反応物 3

HCID 7504BenzylamineHCID 25517Ammonium ChlorideHCID 15380869Methyl 2,2-bis(nitryloxymethyl)-3-nitryloxypropionate

生成物 1

HCID 153808733-nitryloxy-2,2-bis(nitryloxymethyl)propionic acid N-benzylamide収率 73%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

1 g (3.5 mmol) of methyl 3-nitryloxy-2,2-bis(nitryloxymethyl)propionate is heated with 3 ml of benzylamine and 100 ml of ammonium chloride for 3 hours at 130° C., cooled, taken up in 50 ml of chloroform and washed in sequence with water, dilute hydrochloric acid, aqueous bicarbonate solution and again with water. The crude product obtained after evaporating off the solvent is purified column chromatographically. 3-nitryloxy-2,2-bis(nitryloxymethyl)propionic acid N-benzylamide is obtained as a colourless oil. Yield: 73%.

後処理

  1. temperaturecooled
  2. washwashed in sequence with water, dilute hydrochloric acid, aqueous bicarbonate solution and again with water
  3. customThe crude product obtained
  4. customafter evaporating off the solvent
  5. customis purified column chromatographically

出典と根拠

ORDレコード
ord-437a19c7e9c648319fc4ffaaba30cfb3
出典データセット
uspto-grants-2002_04
特許番号
US06365611B1

反応ノート

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