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Iodoethane → 3-Dibenzylamino-6,7-difluoro-1-ethyl-1H-quinazoline-2,4-dione

HRID 10315
ノート
印刷プレビュー

反応式

HRID 10315 の反応式
[CH2:1]([N:8]([CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[N:9]1[C:18](=[O:19])[C:17]2[C:12](=[CH:13][C:14]([F:21])=[C:15]([F:20])[CH:16]=2)[NH:11][C:10]1=[O:22])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH2:32](I)[CH3:33]>CN(C)C=O>[CH2:23]([N:8]([CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[N:9]1[C:18](=[O:19])[C:17]2[C:12](=[CH:13][C:14]([F:21])=[C:15]([F:20])[CH:16]=2)[N:11]([CH2:32][CH3:33])[C:10]1=[O:22])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
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 6340IodoethaneHCID 24758Sodium hydrideHCID 219790003-Dibenzylamino-6,7-difluoro-1H-quinazoline-2,4-dione

生成物 1

HCID 219794283-Dibenzylamino-6,7-difluoro-1-ethyl-1H-quinazoline-2,4-dione収率 73.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A solution of 3-dibenzylamino-6,7-difluoro-1H-quinazoline-2,4-dione (Example 16) (0.43 g, 1.1 mmol) in 10 mL of N,N-dimethylformamide is added to a suspension of sodium hydride (0.05 g, 1.3 mmol) in 10 mL of N,N-dimethylformamide and stirred for 30 minutes. Ethyl iodide (0.13 mL, 1.6 mmol) is added, and the mixture is stirred at 25° C. for 18 hours. The reaction is quenched with 1 mL of water and concentrated in vacuo. The residue is dissolved in chloroform, washed with water, brine, and dried over magnesium sulfate. The solution is concentrated and purified via chromatography (SiO2, CHCl3) to give 0.34 g of the title compound as a solid, mp 133–135° C., MS CI, m/z 422 (MH+).

後処理

  1. stirringthe mixture is stirred at 25° C. for 18 hours
  2. customThe reaction is quenched with 1 mL of water
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue is dissolved in chloroform
  5. washwashed with water, brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationThe solution is concentrated
  8. custompurified via chromatography (SiO2, CHCl3)

出典と根拠

ORDレコード
ord-de33f49a4f9a4548b0cd9c65b986092f
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07094780B1

反応ノート

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