Urea → HCID 178488789、化合物

HRID 1380508ノート

反応式

HRID 1380508 の反応式
[NH2:1][C:2]([NH2:4])=[O:3].CC[O-].[Na+].CN(C)[CH:11]=[C:12]([C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=1)[C:13](=O)[CH3:14]>C(O)C>[CH3:23][O:22][C:19]1[CH:20]=[CH:21][C:16]([C:12]2[C:13]([CH3:14])=[N:1][C:2](=[O:3])[NH:4][CH:11]=2)=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 1176UreaHCID 2723922Sodium ethoxideHCID 539901024-Dimethylamino-3-(4-methoxyphenyl)-3-buten-2-one

生成物 1

HCID 178488789HCID 178488789、化合物収率 49.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

24.4 g of urea and 120 ml of a 25 percent ethanolic solution of sodium ethylate are added to a solution of 40.0 g of 4-dimethylamino-3-(4-methoxyphenyl)-3-buten-2-one in 120 ml of ethanol. The mixture is heated at the reflux temperature for 8 hours, then cooled to 0° C., and the reaction product is filtered off with suction and washed with cold ethanol. The residue is dissolved in water and, while cooling in ice, is neutralised with dilute hydrochloric acid. The precipitated product is filtered off with suction, washed with water and dried. 19.5 g of 5-(4-methoxyphenyl)-4-methyl-2-(1H)-pyrimidinone are obtained. Melting point 210° C.

後処理

  1. temperatureThe mixture is heated at the reflux temperature for 8 hours
  2. filtrationthe reaction product is filtered off with suction
  3. washwashed with cold ethanol
  4. dissolutionThe residue is dissolved in water
  5. temperaturewhile cooling in ice
  6. filtrationThe precipitated product is filtered off with suction
  7. washwashed with water
  8. customdried

出典と根拠

ORDレコード
ord-c13d2d9c19694666ab04d374bef008a8
出典データセット
uspto-grants-1986_04
特許番号
US04582834

反応ノート

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