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3-(2,6-Bis-benzyloxy-5-ethyl-pyrimidine-4-carbonyl)-5-methyl-benzonitrile → 3-(5-ethyl-2,4-dioxo-1H-pyrimidine-6-carbonyl)-5-methyl-benzonitrile

HRID 426120
ノート
印刷プレビュー

反応式

HRID 426120 の反応式
C([O:8][C:9]1[N:14]=[C:13]([C:15]([C:17]2[CH:18]=[C:19]([CH:22]=[C:23]([CH3:25])[CH:24]=2)[C:20]#[N:21])=[O:16])[C:12]([CH2:26][CH3:27])=[C:11]([O:28]CC2C=CC=CC=2)[N:10]=1)C1C=CC=CC=1>C(O)C.C1COCC1.[Pd]>[CH2:26]([C:12]1[C:11](=[O:28])[NH:10][C:9](=[O:8])[NH:14][C:13]=1[C:15]([C:17]1[CH:18]=[C:19]([CH:22]=[C:23]([CH3:25])[CH:24]=1)[C:20]#[N:21])=[O:16])[CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 1

HCID 591847853-(2,6-Bis-benzyloxy-5-ethyl-pyrimidine-4-carbonyl)-5-methyl-benzonitrile

生成物 1

HCID 596868563-(5-ethyl-2,4-dioxo-1H-pyrimidine-6-carbonyl)-5-methyl-benzonitrile収率 738.8%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

3-(2,6-Bis-benzyloxy-5-ethyl-pyrimidine-4-carbonyl)-5-methyl-benzonitrile (41) (4.5 g, 9.7 mmol) in anhydrous ethanol (30 ml) and THF (30 ml) was stirred with 10% palladium on carbon (250 mg) under an atmosphere of hydrogen. After 1.5 hr, the mixture was filtered through celite pad and the filtrate was evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent, chloroform:methanol (95:5)) to afford 20.3 g (84%) of a white solid; m.p. 253-254° C.; 1H NMR (200 MHz, DMSO-d6) δ: 0.84 (3H, t, J=7.0 Hz), 1.96 (2H, q, J=7.0 Hz), 2.45 (3H, s), 8.06 (1H, s), 8.11 (1H, s), 8.33 (1H, s), 11.05 (1H, s), 8.28 (1H, s); m/z (EI): 283 (M+).

後処理

  1. filtrationthe mixture was filtered through celite pad
  2. customthe filtrate was evaporated in vacuo
  3. customThe residue was purified by silica gel column chromatography (eluent, chloroform:methanol (95:5))

出典と根拠

ORDレコード
ord-6fb824d0be97411db0a53e7a96601e44
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08106064B2

反応ノート

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