1,1'-Carbonyldiimidazole → 1-(2-ethoxyethyl)-3-ethyl-1H-pyrazolo[4,3-d]pyrimidine-5,7(4H,6H)-dione

HRID 1896199

反応式

HRID 1896199 の反応式
[C:1](N1C=CN=C1)(N1C=CN=C1)=[O:2].[NH2:13][C:14]1[C:15]([CH2:27][CH3:28])=[N:16][N:17]([CH2:22][CH2:23][O:24][CH2:25][CH3:26])[C:18]=1[C:19]([NH2:21])=[O:20]>C(#N)C>[CH2:25]([O:24][CH2:23][CH2:22][N:17]1[C:18]2[C:19](=[O:20])[NH:21][C:1](=[O:2])[NH:13][C:14]=2[C:15]([CH2:27][CH3:28])=[N:16]1)[CH3:26]

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 577445394-amino-1-(2-ethoxyethyl)-3-ethyl-1H-pyrazole-5-carboxamide

生成物 1

HCID 566051951-(2-ethoxyethyl)-3-ethyl-1H-pyrazolo[4,3-d]pyrimidine-5,7(4H,6H)-dione収率 87.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
50 °C

実験手順

A mixture of carbonyldiimidazole (12.3 g, 76.1 mmol) in acetonitrile (123 mL) was warmed to 50° C. The 4-amino-1-(2-ethoxyethyl)-3-ethyl-1H-pyrazole-5-carboxamide prepared in step 3 (13.2 g, 58 mmol) was added to the mixture over a period of one hour and the temperature of the mixture was increased to 75° C. during the addition. The mixture was then cooled and stirred overnight. The mixture was cooled in an ice bath and filtered. The filter cake was rinsed with water and dried to provide 12.8 g of the title compound.

後処理

  1. temperaturethe temperature of the mixture was increased to 75° C. during the addition
  2. temperatureThe mixture was then cooled
  3. temperatureThe mixture was cooled in an ice bath
  4. filtrationfiltered
  5. washThe filter cake was rinsed with water
  6. customdried

出典と根拠

ORDレコード
ord-0dcd4fbb7f694b759eb4b342704eb1e1
出典データセット
uspto-grants-2013_08
特許番号
US08518956B2

関連ノート

読み込み中…