Methyl iodide → HCID 135471382、化合物

HRID 2406200ノート

反応式

HRID 2406200 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[S:12])[NH:6][C:5]2=[O:13].[CH3:14][O-].[Na+].IC>CN(C=O)C.CO>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([S:12][CH3:14])[NH:6][C:5]2=[O:13]

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 8408566-Bromo-2-thioxo-2,3-dihydroquinazolin-4(1H)-oneHCID 10942334Sodium Methoxide

生成物 1

HCID 135471382HCID 135471382、化合物収率 90.3%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of compound 4a (8.43 g, 32.8 mmol) in 130 mL of DMF was added a solution sodium methoxide (0.50 M, 32.8 mmol) in methanol (65.6 mL) and the mixture was stirred at room temperature for 15 minutes. Iodomethane (2.04 mL, 32.8 mmol) was added and the reaction mixture was stirred at room temperature for 22 hours. The solvents were evaporated under reduced pressure and the remaining solid was dissolved in 500 mL of EtOAc and washed with 400 mL of a saturated solution of aqueous NaHCO3. The organic layer was dried over MgSO4, concentrated under reduced pressure and precipitated from 50 mL of ethyl alcohol, to give 5a as a white solid (8.03 g, 90%). mp: 230° C.,

後処理

  1. stirringthe reaction mixture was stirred at room temperature for 22 hours
  2. customThe solvents were evaporated under reduced pressure
  3. dissolutionthe remaining solid was dissolved in 500 mL of EtOAc
  4. washwashed with 400 mL of a saturated solution of aqueous NaHCO3
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated under reduced pressure
  7. customprecipitated from 50 mL of ethyl alcohol

出典と根拠

ORDレコード
ord-bfb3206fe85c4686a92698a7c17996f2
出典データセット
uspto-grants-2014_08
特許番号
US08809355B2

反応ノート

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