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

HRID 63120

反応式

HRID 63120 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  1. filtrationthe solid was collected by filtration
  2. customdried

出典と根拠

ORDレコード
ord-8b9970a145f54e7f8cdb43222681458b
出典データセット
uspto-grants-2016_09
特許番号
US09447051B2

関連ノート

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