Oxalic Acid → HCID 135577947、化合物

HRID 2165720ノート

反応式

HRID 2165720 の反応式
C(O)(=O)C(O)=O.C(C(CC)C(O)=O)C.[C:15]([NH:18][C:19]1[NH:20][C:21](=[O:35])[C:22]([CH2:32][CH:33]=[O:34])=[C:23]([N:25]([C:29](=[O:31])[CH3:30])[C:26](=[O:28])[CH3:27])[N:24]=1)(=[O:17])[CH3:16].C(=O)(O)[O-].[Na+]>ClCCl>[C:15]([NH:18][C:19]1[NH:20][C:21](=[O:35])[C:22]([CH2:32][CH:33]=[O:34])=[C:23]([N:25]([C:29](=[O:31])[CH3:30])[C:26](=[O:28])[CH3:27])[N:24]=1)(=[O:17])[CH3:16]

参加物

5

反応物 3

HCID 971Oxalic AcidHCID 516892Sodium BicarbonateHCID 136364561HCID 136364561、化合物

生成物 1

HCID 135577947HCID 135577947、化合物収率 46.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A slurry of Silica Gel 60 (6.0 g, Merck μ7734, 70-230 mesh) and aqueous oxalic acid (10%) (0.6 ml) in dichlormethane (12 ml) was stirred for 15 minutes. 2-(2-acetylamino-4-diacetylamino-1,6-dihydro-6-oxo-5-pyrimidinyl)acetaldehyde diethyl acetate (1.0 g, 2.7 mmol) was added and the mixture was stirred for 18 hours. Sodium bicarbonate (0.2 g, 2.4 mmol) was added and after 10 minutes the slurry was filtered and washed with ethyl acetate. The filtrates and wash were combined and spin evaporated in vacuo to give 0.37 g (46% of theory) of 2-(2-acetylamino-4-diacetylamino-1,6-dihydro-6-oxo-5-pyrimidinyl)acetaldehyde. The analytical sample was prepared by recrystallization from acetone to give 0.21 g (26% of theory), mp 169°-170° C.)

後処理

  1. filtrationwas filtered
  2. washwashed with ethyl acetate
  3. washThe filtrates and wash
  4. customspin evaporated in vacuo

出典と根拠

ORDレコード
ord-a33e37df03444055a39b479029c025aa
出典データセット
uspto-grants-1990_07
特許番号
US04940713

反応ノート

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