1,3-Dimethyl-2-imidazolidinone → HCID 136403422、化合物

HRID 1613220ノート

反応式

HRID 1613220 の反応式
[N+:1]([N:4]=[C:5]1[NH:10][CH2:9][CH2:8][CH2:7][NH:6]1)([O-:3])=[O:2].[CH:11]([O-:16])([O-])[O:12][CH2:13][CH3:14].CN1[CH2:22][CH2:21]N(C)C1=O>>[CH2:21]([O:16][CH:11]([O:12][CH2:13][CH3:14])[N:6]1[CH2:7][CH2:8][CH2:9][NH:10][C:5]1=[N:4][N+:1]([O-:3])=[O:2])[CH3:22]

参加物

4

反応物 3

HCID 66611,3-Dimethyl-2-imidazolidinoneHCID 53630039EthylorthoformateHCID 13624905053360-90-0

生成物 1

HCID 136403422HCID 136403422、化合物

実験手順

A mixture of 10 g of 2-nitroiminohexahydropyrimidine, 12.4 g of ethyl orthoformate, 10 ml of 1,3-dimethyl-2-imidazolidinone was heated under reflux for 2.0 hours 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 oil was purified by column chromatography [silica gel, eluent: hexane/ethyl acetate (1:2)] to obtain 2.3 g of 1-diethoxymethyl-2-nitroiminohexahydropyrimidine. Typical examples of the compounds of the formula (2) which could be prepared according to the procedures similar to those of Examples 9 to 14 are shown in Table 3.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 2.0 hours
  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 oil was purified by column chromatography [silica gel, eluent: hexane/ethyl acetate (1:2)]

出典と根拠

ORDレコード
ord-444122a55ba344a0b00029821c3b15ab
出典データセット
uspto-grants-1993_03
特許番号
US05192778

反応ノート

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