Methyl iodide → HCID 14638935、化合物

HRID 877018ノート

反応式

HRID 877018 の反応式
[CH3:1][C:2]1[S:12][C:5]2[NH:6][C:7](=O)[NH:8][C:9](=[O:10])[C:4]=2[CH:3]=1.[C:13]([O-:16])([O-])=O.[K+].[K+].[CH3:19]I>CN(C=O)C.O>[CH3:19][N:6]1[C:5]2[S:12][C:2]([CH3:1])=[CH:3][C:4]=2[C:9](=[O:10])[N:8]([CH3:7])[C:13]1=[O:16]

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 127242076-Methylthieno[2,3-d]pyrimidine-2,4(1H,3H)-dione

生成物 1

HCID 14638935HCID 14638935、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of Step 3 intermediate (13.5 g, 74.17 mmol) in dry DMF (148 ml) was added anhydrous K2CO3 (51.25 g, 370.85 mmol) and the mixture was stirred at room temperature for 1 h. Methyl iodide (34.74 g, 244.78 mmol) was added slowly with stirring and further stirred at room temperature for 24 h. The reaction mixture was diluted with water and the solid precipitated out was filtered, washed with water and dried to give 12.6 gm of the product as a brown solid; 1H NMR (300 MHz, DMSO-d6) δ 2.42 (s, 3H), 3.22 (s, 3H), 3.42 (s, 3H), 6.90 (s, 1H).

後処理

  1. stirringwith stirring
  2. stirringfurther stirred at room temperature for 24 h
  3. customthe solid precipitated out
  4. filtrationwas filtered
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-22d7d3ce66aa47559346210f95dad6a4
出典データセット
uspto-grants-2015_03
特許番号
US08987278B2

反応ノート

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