Sulfuric Acid → HCID 136403421、化合物

HRID 1613219ノート

反応式

HRID 1613219 の反応式
[CH:1]([O-:5])([O-])[O:2][CH3:3].[CH3:6]N1CCN(C)C1=O.S(=O)(=O)(O)O.[N+:19]([N:22]=[C:23]1[NH:28][CH2:27][CH2:26][CH2:25][NH:24]1)([O-:21])=[O:20]>>[CH3:6][O:5][CH:1]([O:2][CH3:3])[N:24]1[CH2:25][CH2:26][CH2:27][NH:28][C:23]1=[N:22][N+:19]([O-:21])=[O:20]

参加物

5

反応物 4

HCID 1118Sulfuric AcidHCID 66611,3-Dimethyl-2-imidazolidinoneHCID 53629101MethylorthoformateHCID 13624905053360-90-0

生成物 1

HCID 136403421HCID 136403421、化合物

実験手順

20.0 g of methyl orthoformate was dropped in about 1.5 hours in a mixture of 10 g of 2-nitroiminohexahydropyrimidine, 20 ml of 1,3-dimethyl-2-imidazolidinone and 0.05 g of sulfuric acid at 150° C., followed by heating under reflux for further 1 hour while removing the resultant distillate by means of the Dean-Stark trap. After cooling to room temperature, the mixture was poured into water, and extracted with ethyl acetate. After washing with water, the extract was dried with anhydrous magnesium sulfate, after which the solvent was distilled off under reduced pressure. The resultant oily substance was purified by column chromatography [silica gel, eluant: hexane/ethyl acetate (1:2)] to give 1.5 g of 1-dimethoxymethyl-2-nitroiminohexahydropyrimidine.

後処理

  1. temperatureby heating
  2. temperatureunder reflux for further 1 hour
  3. customwhile removing the resultant distillate by means of the Dean-Stark trap
  4. additionthe mixture was poured into water
  5. extractionextracted with ethyl acetate
  6. washAfter washing with water
  7. dry with materialthe extract was dried with anhydrous magnesium sulfate
  8. distillationafter which the solvent was distilled off under reduced pressure
  9. customThe resultant oily substance was purified by column chromatography [silica gel, eluant: hexane/ethyl acetate (1:2)]

出典と根拠

ORDレコード
ord-563d7e93a7d145ac8691b969ca943b54
出典データセット
uspto-grants-1993_03
特許番号
US05192778

反応ノート

読み込み中…