反応 #895

反応方程式

sodium thiomethoxide

4,6-dichloro-2-(phenylmethoxy)pyrimidine

→

4-chloro-6-methylthio-2-(phenylmethoxy)pyrimidine

溶媒

THF

反応条件

後処理

1. 1
   その他to react for 2 hours
2. 2
   その他the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
3. 3
   洗浄The organic layer was washed with aqueous saturated sodium chloride
4. 4
   乾燥dried over anhydrous sodium sulfate
5. 5
   濃縮concentrated
6. 6
   その他purified on a silica gel column

実験手順

Aqueous sodium thiomethoxide (15%, 2.75 g, 0.0059×1.0 mol) was added dropwise in 4,6-dichloro-2-(phenylmethoxy)pyrimidine (Compound No. II-26) (1.5 g, 0.0059 mol) dissolved in THF at room temperature. After allowed to react for 2 hours, the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated, then purified on a silica gel column to obtain 4-chloro-6-methylthio-2-(phenylmethoxy)pyrimidine (Compound No. II-15) as an intermediate.

出典