Acetyl chloride → (Methylnitramino)methylacetate

HRID 1285556

反応式

HRID 1285556 の反応式
[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]

参加物

4

反応物 2

HCID 6367Acetyl chlorideHCID 119262Methanol, (methylnitramino)-

生成物 1

HCID 147637(Methylnitramino)methylacetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d39d401e85144d65ac55ddcdc5ccb1da
出典データセット
uspto-grants-1986_01
特許番号
US04567296

関連ノート

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