Acetyl chloride → (Methylnitramino)methylacetate

HRID 2081919

반응식

HRID 2081919 반응식
[N+:1]([N:4]([CH3:7])[CH2:5][OH:6])([O-:3])=[O:2].[C:8](Cl)(=[O:10])[CH3:9]>ClCCl>[C:8]([O:6][CH2:5][N:4]([N+:1]([O-:3])=[O:2])[CH3:7])(=[O:10])[CH3:9]

참가 물질

4

실험 절차

To a stirred mixture of 10.6 g of 2-nitro-2-aza-1-propanol and 25 ml of dichloromethane under a nitrogen atmosphere was added dropwise and with ice-cooling 12 g of acetyl chloride. The cooling bath was removed and the mixture was slowly heated to reflux. After 3 hours the solution was allowed to cool and was then triturated with 50 ml of ice water. The organic phase was separated, dried (MgSO4), and distilled. The product 2-nitro-2-azapropyl acetate had b.p. 56°-57° C. at 0.07 mm Hg.

후처리

  1. additionwas added dropwise and with ice-
  2. customThe cooling bath was removed
  3. temperaturethe mixture was slowly heated to reflux
  4. temperatureto cool
  5. customwas then triturated with 50 ml of ice water
  6. customThe organic phase was separated
  7. dry with materialdried (MgSO4)
  8. distillationdistilled

출처 및 근거

ORD 기록
ord-87c26324ad1d4bc7b0a8c702dd35ba7f
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05186770

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