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

HRID 840192노트

반응식

HRID 840192 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-437a19c7e9c648319fc4ffaaba30cfb3
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06365611B1

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