反应详情

To a solution of 1-(4-amino-6-(methylthio)-1,3,5-triazin-2-yl)ethanol (203 mg) in dry tetrahydrofuran (8 mL) was added 2-chlorophenol (0.122 mL) and triphenylphosphine (314 mg) followed by diisopropyl azodicarboxylate ((0.233 mL) dropwise. The solution was stirred at room temperature for 80 min then was concentrated in vacuo, dissolved in ethyl acetate (40 mL) and washed with 1N sodium hydroxide solution (2×40 mL), dried over sodium sulfate and concentrated to give a yellow oil. Purification by SCX chromatography eluting with a 1:1 mixture of dichloromethane-methanol then 2N ammonia in 1:1 mixture of dichloromethane-methanol followed by flash column chromatography, with 1% acetonirile in dichloromethane to give the title compound (207 mg).

1. concentrationthen was concentrated in vacuo
2. dissolutiondissolved in ethyl acetate (40 mL)
3. washwashed with 1N sodium hydroxide solution (2×40 mL)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customto give a yellow oil
7. customPurification by SCX chromatography
8. washeluting with a 1:1 mixture of dichloromethane-methanol
9. addition2N ammonia in 1:1 mixture of dichloromethane-methanol