Acetic Acid → HCID 178474467、化合物

HRID 1651054

反応式

HRID 1651054 の反応式
[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]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 178474468HCID 178474468、化合物

生成物 1

HCID 178474467HCID 178474467、化合物収率 77%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-c1f5350ef8f04e10be86cca0e0b0f609
出典データセット
uspto-grants-1990_05
特許番号
US04927828

関連ノート

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