Potassium Carbonate → 5-[4-(4-Chlorophenyl)-1-piperazinyl]-6-methyl-2,4-(1H, 3H)-pyrimidinedione

HRID 371473

反応式

HRID 371473 の反応式
Br[C:2]1[C:3](=[O:10])[NH:4][C:5](=[O:9])[NH:6][C:7]=1[CH3:8].[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[CH:14][CH:13]=1.O.O.[F-].[K+].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[Cl:11][C:12]1[CH:13]=[CH:14][C:15]([N:18]2[CH2:23][CH2:22][N:21]([C:2]3[C:3](=[O:10])[NH:4][C:5](=[O:9])[NH:6][C:7]=3[CH3:8])[CH2:20][CH2:19]2)=[CH:16][CH:17]=1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 847572,4(1H,3H)-Pyrimidinedione, 5-bromo-6-methyl-HCID 974781-(4-Chlorophenyl)piperazineHCID 23708904Potassium fluoride dihydrate

生成物 1

HCID 544234455-[4-(4-Chlorophenyl)-1-piperazinyl]-6-methyl-2,4-(1H, 3H)-pyrimidinedione収率 18.9%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture of 20.50 g (0.100 mole) of 5-bromo-6-methyl-2,4(1H, 3H)pyrimidinedione, 26.96 g (0.100 mole of 1-(4-chlorophenyl)-piperazine, 10.35 g (0.110 mole) of potassium fluoride dihydrate and 41.40 g (0.300 mole) of potassium carbonate in 200 ml of dimethylsulfoxide was heated at 80° for 72 hours. The reaction mixture was cooled and poured into 1 l of ice water. The solid was collected, washed with water, and recrystallized from ethanol to give 6.05 g of the product as a dull yellow solid.

後処理

  1. temperaturewas heated at 80° for 72 hours
  2. temperatureThe reaction mixture was cooled
  3. customThe solid was collected
  4. washwashed with water
  5. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-cd3a279158e743fc8ca4bfc331dc0ccc
出典データセット
uspto-grants-1985_07
特許番号
US04532240

関連ノート

読み込み中…