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Water → 3-[2-[4-(4-Fluorobenzoyl)piperidin-1-yl]ethyl]-1-methylthieno[3,4-d]pyrimidine-2,4-dione

HRID 1762830
ノート
印刷プレビュー

反応式

HRID 1762830 の反応式
[F:1][C:2]1[CH:28]=[CH:27][C:5]([C:6]([CH:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][N:16]3[C:21](=[O:22])[C:20]4=[CH:23][S:24][CH:25]=[C:19]4[NH:18][C:17]3=[O:26])[CH2:10][CH2:9]2)=[O:7])=[CH:4][CH:3]=1.[H-].[Na+].[CH3:31]I.O>CN(C)C=O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([CH:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][N:16]3[C:21](=[O:22])[C:20]4=[CH:23][S:24][CH:25]=[C:19]4[N:18]([CH3:31])[C:17]3=[O:26])[CH2:10][CH2:9]2)=[O:7])=[CH:27][CH:28]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 145003983-[2-[4-(4-Fluorobenzoyl)piperidin-1-yl]ethyl]thieno[3,4-d]pyrimidine-2,4-dione

生成物 1

HCID 145004023-[2-[4-(4-Fluorobenzoyl)piperidin-1-yl]ethyl]-1-methylthieno[3,4-d]pyrimidine-2,4-dione

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

The title compound was prepared by dissolving the 3-[2-[4-(4-fluorobenzoyl)piperidin-1-yl]ethyl]thieno[3,4-d]pyrimidine-2,4-dione from Example 10 (1.8 g, 4.6 mmol) in 10 ml of dimethylformamide at 0° C. After treating this solution with NaH (203 mg, 5 mmol) followed by 720 mg (5 mmol) of methyl iodide, the mixture was stirred at room temperature for 24 hours. The reaction was poured into water and extracted with CH2Cl2. The combined extracts were washed with water and brine and dried over MgSO4. Solvent removal produced a crude product which was purified by flash silica gel chromatography using 2% MeOH/CH2Cl2. The title compound was crystallized from CH2Cl2 /hexane to give a white solid (1.04 g, 54% yield), mp 176°-178° C.

後処理

  1. extractionextracted with CH2Cl2
  2. washThe combined extracts were washed with water and brine
  3. dry with materialdried over MgSO4
  4. customSolvent removal
  5. customproduced a crude product which

出典と根拠

ORDレコード
ord-493b6785d3d04d8ea6a84bf03b0b9e4f
出典データセット
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04835157

反応ノート

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