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

HRID 1896199

반응식

HRID 1896199 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0dcd4fbb7f694b759eb4b342704eb1e1
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518956B2

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