Acetic Acid → HCID 178474467, 화합물

HRID 1651054

반응식

HRID 1651054 반응식
[C:1]([NH:4][C:5]1[N:6]=[C:7]([OH:29])[C:8]2[CH:14]=[C:13]([CH:15]=[CH:16][C:17]3[CH:22]=[CH:21][C:20]([C:23]([O:25]C(=O)C)=[O:24])=[CH:19][CH:18]=3)[CH:12]=[N:11][C:9]=2[N:10]=1)(=[O:3])[CH3:2].[OH-].[Na+].C(O)(=O)C>O>[C:1]([NH:4][C:5]1[N:6]=[C:7]([OH:29])[C:8]2[CH:14]=[C:13]([CH:15]=[CH:16][C:17]3[CH:22]=[CH:21][C:20]([C:23]([OH:25])=[O:24])=[CH:19][CH:18]=3)[CH:12]=[N:11][C:9]=2[N:10]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 178474468HCID 178474468, 화합물

생성물 1

HCID 178474467HCID 178474467, 화합물수율 77%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a suspension of 0.95 g of 2-acetamido-4- hydroxy-6-[2-(4-acetoxycarbonylphenyl)ethenyl]pyrido[2,3-d]pyrimidine in 50 mL of water was added 1N aqueous sodium hydroxide until a homogenous solution was obtained. Acidification with acetic acid resulted in the formation of a yellow precipitate which was collected by filtration. The filter cake was washed sequentially with water, methanol, acetone and ether. The residual solid was recrystallized from DMF to give 0.65 g (77%) of 2-acetamido-4-hydroxy-6-[2-(4-carboxyphenyl)-ethenyl]pyrido[2,3-d]pyrimidine, as a microcrystalline yellow solid, mp>300° C.; NMR (TFA-d ) delta 2.5 (s, 3H), 6.85, 7.32 (AB q, 2H, J=12 Hz), 7.45, 8.18 (AB q, 4H, J=9 Hz), 8.65 (s, 1H), 9.02 (s, 1H); IR (Nujol) 3300-2200 (br), 1685, 1655, 1630, 1600, 1565 cm-1. MS: Calc'd. for C 18 H14N4O4 : 350. Found: m/e 350 (base), 308

후처리

  1. customwas obtained
  2. filtrationwas collected by filtration
  3. washThe filter cake was washed sequentially with water, methanol, acetone and ether
  4. customThe residual solid was recrystallized from DMF

출처 및 근거

ORD 기록
ord-c1f5350ef8f04e10be86cca0e0b0f609
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04927828

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