4-Methyl-2-(methylsulfanyl)-5-{[(methylsulfanyl)methoxy]methyl}pyrimidine → 5-[(Chloromethoxy)methyl]-4-methyl-2-(methylsulfanyl)pyrimidine
反応式
S(Cl)(Cl)(=O)=O.[CH3:6][S:7][C:8]1[N:13]=[C:12]([CH3:14])[C:11]([CH2:15][O:16][CH2:17][Cl:18])=[CH:10][N:9]=1.CSC1N=C(C)C(COCSC)=CN=1>ClCCl>[CH3:6][S:7][C:8]1[N:13]=[C:12]([CH3:14])[C:11]([CH2:15][O:16][CH2:17][Cl:18])=[CH:10][N:9]=1参加物
4
反応条件
- 温度
- -3 °C
実験手順
2-Methylthio-4-methyl-5-(chloromethyloxymethyl)pyrimidine Sulfuryl chloride (2.8 mmol) in dry dichloromethane (5 ml) was added dropwise over 15 minutes at -3° C. to a solution of 2-methylthio-4-methyl-5-(methylthiomethyloxy)methylpyrimidine (2.8 mmol) in dry dichloromethane (10 ml). The mixture was stirred at -3° C. for 10 minutes before the solution was evaporated at reduced pressure. The crude product (0.60 g, 98%) was used for alkylation in Example 10 without any further purification. 1H NMR (CDCl3): δ2.64 (4-CH3 and SCH3), 4.73 (CH2), 5.50 (CH2), 8.47 (H-6).
後処理
- customwas evaporated at reduced pressure
- customThe crude product (0.60 g, 98%) was used for alkylation in Example 10 without any further purification
出典と根拠
- ORDレコード
- ord-62c3c87e492147bb971788be64056faf
- 出典データセット
- uspto-grants-1985_09
- 特許番号
- US04539324
反応ノート
読み込み中…