Oxalic Acid → HCID 135577947, 화합물

HRID 2165720노트

반응식

HRID 2165720 반응식
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]

참가 물질

5

반응물 3

HCID 971Oxalic AcidHCID 516892Sodium BicarbonateHCID 136364561HCID 136364561, 화합물

생성물 1

HCID 135577947HCID 135577947, 화합물수율 46.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.)

후처리

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

출처 및 근거

ORD 기록
ord-a33e37df03444055a39b479029c025aa
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04940713

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