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Pyridine → 5-(6-Acetoxy-2.5,7,8-tetramethvlchroman-2-carboxamido)-6-amino-3-methyl-1-phenyl-2,4 (1H, 3H)-pyrimidinedione

HRID 399423
ノート
印刷プレビュー

反応式

HRID 399423 の反応式
[NH2:1][C:2]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6](=[O:14])[N:5]([CH3:15])[C:4](=[O:16])[C:3]=1[NH:17][C:18]([C:20]1([CH3:34])[CH2:29][CH2:28][C:27]2[C:22](=[C:23]([CH3:33])[C:24]([CH3:32])=[C:25]([OH:31])[C:26]=2[CH3:30])[O:21]1)=[O:19].N1C=CC=CC=1.[C:41](OC(=O)C)(=[O:43])[CH3:42]>ClCCl>[C:41]([O:31][C:25]1[C:26]([CH3:30])=[C:27]2[C:22](=[C:23]([CH3:33])[C:24]=1[CH3:32])[O:21][C:20]([CH3:34])([C:18]([NH:17][C:3]1[C:4](=[O:16])[N:5]([CH3:15])[C:6](=[O:14])[N:7]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[C:2]=1[NH2:1])=[O:19])[CH2:29][CH2:28]2)(=[O:43])[CH3:42]
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 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 9825688N-(4-amino-1-methyl-2,6-dioxo-3-phenylpyrimidin-5-yl)-6-hydroxy-2,5,7,8-tetramethyl-3,4-dihydrochromene-2-carboxamide

生成物 1

HCID 572790375-(6-Acetoxy-2.5,7,8-tetramethvlchroman-2-carboxamido)-6-amino-3-methyl-1-phenyl-2,4 (1H, 3H)-pyrimidinedione収率 87%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

The compound of Example 1 (1.77 g, 3.80 mmol) and pyridine (0.154 mL, 1.90 mmol) were dissolved in dichloromethane (30 mL). To the resultant solution was added dropwise acetic anhydride (0.714 mL, 7.60 mmol) under ice cooling. The resultant reaction mixture was stirred overnight at room temperature, washed with 1N hydrochloric acid and 10% aqueous solution of sodium chloride successively, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was suspended in ethyl acetate and filtered to give the title compound (yield 87%).

後処理

  1. customThe resultant reaction mixture
  2. washwashed with 1N hydrochloric acid and 10% aqueous solution of sodium chloride successively
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-c9b20a5e69464fa0a5a66a00e811cefa
出典データセット
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05821247

反応ノート

読み込み中…

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