Acetic Acid → 5,6-dimethyl-2-(methylsulfanyl)pyrimidin-4(1h)-one

HRID 63120

반응식

HRID 63120 반응식
[CH3:1][C:2]1[C:3](=[O:10])[NH:4][C:5](=[S:9])[NH:6][C:7]=1[CH3:8].[OH-].[Na+].CI.[C:15](O)(=O)C>O>[CH3:1][C:2]1[C:3](=[O:10])[NH:4][C:5]([S:9][CH3:15])=[N:6][C:7]=1[CH3:8]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 27362495,6-Dimethyl-2-thiouracil

생성물 1

HCID 1354949705,6-dimethyl-2-(methylsulfanyl)pyrimidin-4(1h)-one수율 64%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred solution of 5,6-dimethyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (10.0 g, 64.0 mmol, Example 1, Step A) and sodium hydroxide (10.0 g, 260.0 mmol) in water (150 mL) at ambient temperature was added methyl iodide (15.0 g, 320.0 mmol), and the reaction mixture was stirred at ambient temperature overnight. Then the reaction mixture was acidified with acetic acid (50 mL), and the solid was collected by filtration and dried to afford 7.0 g (64%) of the titled compound as a white solid. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.87 (s, 3H), 2.18 (s, 3H), 2.45 (s, 3H), 12.38 (bs, 1H).

후처리

  1. filtrationthe solid was collected by filtration
  2. customdried

출처 및 근거

ORD 기록
ord-8b9970a145f54e7f8cdb43222681458b
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447051B2

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