Guanidine Nitrate → 7-Amino-1,3-diethyl-pyrimido[4,5-d]pyrimidine-2,4-dione

HRID 476917

반응식

HRID 476917 반응식
[Na].[N+]([O-])(O)=O.[NH2:6][C:7]([NH2:9])=[NH:8].N[C:11]1[N:16]([CH2:17][CH3:18])[C:15](=[O:19])[N:14]([CH2:20][CH3:21])[C:13](=[O:22])[C:12]=1[CH:23]=O>C(O)C>[NH2:8][C:7]1[N:9]=[C:11]2[N:16]([CH2:17][CH3:18])[C:15](=[O:19])[N:14]([CH2:20][CH3:21])[C:13](=[O:22])[C:12]2=[CH:23][N:6]=1

참가 물질

5

반응물 3

HCID 10481Guanidine NitrateHCID 34600936-Amino-1,3-diethyl-5-formyluracilHCID 5360545Sodium

생성물 1

HCID 148548837-Amino-1,3-diethyl-pyrimido[4,5-d]pyrimidine-2,4-dione수율 87%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.92 g of sodium was dissolved in 50 ml of absolute ethanol, and 6.40 g (53 mmol) of guanidine nitrate was added thereto. The solution was stirred for 10 minutes and filtered with Celite filter aid. 0.98 g (4.6 mmol) of 6-amino-1,3-diethyl-5-formyluracil was added to the filtrate and the reaction mixture was refluxed for 24 hours. After removal of the solvent under reduced pressure, 30 ml of water was added thereto. The crystalline precipitate was filtered off and recrystallized from ethanol to give 0.94 g of 7-amino-1,3-diethyl-pyrimido[4,5-d]pyrimidine-2,4-dione (compound 17) in a 87% yield.

후처리

  1. filtrationfiltered with Celite
  2. filtrationfilter aid
  3. temperaturethe reaction mixture was refluxed for 24 hours
  4. customAfter removal of the solvent under reduced pressure, 30 ml of water
  5. additionwas added
  6. filtrationThe crystalline precipitate was filtered off
  7. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-acdbb86cf79745199c2dfd346727fc0b
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04886807

연결된 노트

불러오는 중…