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

HRID 476917

反応式

HRID 476917 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-acdbb86cf79745199c2dfd346727fc0b
出典データセット
uspto-grants-1989_12
特許番号
US04886807

関連ノート

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