Methyl iodide → HCID 14638935, 화합물

HRID 877018노트

반응식

HRID 877018 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 14638935HCID 14638935, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-22d7d3ce66aa47559346210f95dad6a4
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987278B2

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