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Urea → 5-(1-Methylethyl)-2,4,6(1H,3H,5H)-pyrimidinetrione

HRID 1281084
ノート
印刷プレビュー

反応式

HRID 1281084 の反応式
[CH:1]([CH:4]([C:10]([O:12]CC)=O)[C:5]([O:7]CC)=O)([CH3:3])[CH3:2].C[O-].[Na+].[NH2:18][C:19]([NH2:21])=[O:20]>CO>[CH3:3][CH:1]([CH:4]1[C:5](=[O:7])[NH:21][C:19](=[O:20])[NH:18][C:10]1=[O:12])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1176UreaHCID 12966Diethyl isopropylmalonateHCID 10942334Sodium Methoxide

生成物 1

HCID 818745-(1-Methylethyl)-2,4,6(1H,3H,5H)-pyrimidinetrione収率 69.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
20 °C

実験手順

456 g (2.25 mol) of diethyl isopropylmalonate, 650 ml of a 30% methanolic sodium methoxide solution and 910 ml of methanol are charged to a 2 liter reactor equipped with an anchor stirrer. The mixture is brought to reflux for thirty minutes before adding 135 g (2.25 mol) of urea in the solid form while maintaining the reflux. The reaction mixture at the end of the reaction is a thick white suspension which is brought to dryness by evaporation of the methanol under vacuum. The residue is taken up in 1370 ml of water and then filtered after cooling to 20° C. The filtrate is treated by addition of the amount of hydrochloric acid needed to bring the pH to 2-3, and the precipitate obtained is filtered off under cold conditions and washed with ice-cold water in order to obtain 267 g of 5-(1-methylethyl)pyrimidine-2,4,6(1H,3H,5H)-trione.

後処理

  1. customequipped with an anchor stirrer
  2. temperatureto reflux for thirty minutes
  3. temperaturewhile maintaining the reflux
  4. customis brought to dryness by evaporation of the methanol under vacuum
  5. filtrationfiltered
  6. additionThe filtrate is treated by addition of the amount of hydrochloric acid
  7. customthe precipitate obtained
  8. filtrationis filtered off under cold conditions
  9. washwashed with ice-cold water in order

出典と根拠

ORDレコード
ord-09785d7a12f045d1b73381a2b99553c0
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06452006B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート