Acetyl chloride → (Methylnitramino)methylacetate

HRID 1285556

반응식

HRID 1285556 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

반응물 2

HCID 6367Acetyl chlorideHCID 119262Methanol, (methylnitramino)-

생성물 1

HCID 147637(Methylnitramino)methylacetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred mixture of 10.6 g of 2-nitro-2-azapropanol 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 (MG SO4), 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. customdried (MG SO4)
  8. distillationdistilled

출처 및 근거

ORD 기록
ord-d39d401e85144d65ac55ddcdc5ccb1da
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04567296

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