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

HRID 1896204

반응식

HRID 1896204 반응식
[NH2:1][C:2]1[C:3]([CH2:15][CH3:16])=[N:4][N:5]([CH2:10][CH2:11][O:12][CH2:13][CH3:14])[C:6]=1[C:7]([NH2:9])=[O:8].[C:17](N1C=CN=C1)(N1C=CN=C1)=[O:18]>CN(C)C=O>[CH2:13]([O:12][CH2:11][CH2:10][N:5]1[C:6]2[C:7](=[O:8])[NH:9][C:17](=[O:18])[NH:1][C:2]=2[C:3]([CH2:15][CH3:16])=[N:4]1)[CH3:14]

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 38.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A mixture of 4-amino-1-(2-ethoxyethyl)-3-ethyl-1H-pyrazole-5-carboxamide from step 2 (2.44 g, 10.8 mmol) in N,N-dimethylformamide (40 mL) was treated with carbonyldiimidazole (1.92 g, 11.9 mmol) and heated at 80° C. overnight. The mixture was concentrated in vacuuo and the residue was purified by column chromatography on silica gel using a mixture of ethyl acetate and hexane as the eluent to provide 1.04 g of the title compound. MS (ESI) m/z 253.

후처리

  1. concentrationThe mixture was concentrated in vacuuo
  2. customthe residue was purified by column chromatography on silica gel using
  3. additiona mixture of ethyl acetate and hexane as the eluent

출처 및 근거

ORD 기록
ord-f415cfce77a54f879508131baf452c9c
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518956B2

연결된 노트

불러오는 중…