3-Thiocresol → 1-(3-Tolylsulfenyl)methyl-5-chloropyrimidin-2-one

HRID 247084

反応式

HRID 247084 の反応式
Cl[CH2:2][N:3]1[CH:8]=[C:7]([Cl:9])[CH:6]=[N:5][C:4]1=[O:10].[CH3:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([SH:18])[CH:13]=1.C(N(CC)CC)C>>[C:12]1([CH3:11])[CH:17]=[CH:16][CH:15]=[C:14]([S:18][CH2:2][N:3]2[CH:8]=[C:7]([Cl:9])[CH:6]=[N:5][C:4]2=[O:10])[CH:13]=1

参加物

4

反応物 3

HCID 79303-ThiocresolHCID 8471TriethylamineHCID 201613341-Chloromethyl-5-chloropyrimidin-2-one

生成物 1

HCID 135300961-(3-Tolylsulfenyl)methyl-5-chloropyrimidin-2-one

反応条件

温度
40 °C

実験手順

1-Chloromethyl-5-chloropyrimidin-2-one (see Preparation 15) (1.0 mmol) was added to a mixture of m-thiocresol (1.0 mmol) and triethylamine (1.0 mmol). The mixture was stirred at room temperature for 20 mins and at 40° C. for 20 mins before the solvent was distilled off and the residue triturated with water, extracted into chloroform, dried (MgSO4) and evaporated. The residue was washed with cold acetone (1 ml). The insoluble product was identical with an authentic sample prepared as described in Example 14. Yield: 60 mg, 22%.

後処理

  1. distillationwas distilled off
  2. customthe residue triturated with water
  3. extractionextracted into chloroform
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. washThe residue was washed with cold acetone (1 ml)
  7. customprepared

出典と根拠

ORDレコード
ord-406721d3280f4895bc58b724e66e5d4b
出典データセット
uspto-grants-1987_11
特許番号
US04705791

関連ノート

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