反応 #67685

反応方程式

2-methyl-1-phenylpropan-2-yl 2-((4R,6S)-6-((E)-2-(4-(4-fluorophenyl)-6-isopropyl-2-(N-methylmethylsulfonamido)pyrimidin-5-yl)vinyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate

hydrochloric acid

sodium hydroxide

→

(E)-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl](3R,5S)-3,5-dihydroxyhept-6-enoic acid sodium salt

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他The reaction liquid
2. 2
   温度was cooled to room temperature
3. 3
   workup.WAITover 5 minutes
4. 4
   workup.STIRRINGby stirring for 4 hours
5. 5
   その他Ethyl acetate (250 ml) and purified water (250 ml)
6. 6
   workup.ADDITIONwere added to the reaction liquid
7. 7
   その他the organic layer was separated
8. 8
   洗浄washed with saturated sodium chloride (150 ml)
9. 9
   乾燥dried over anhydrous sodium sulfate
10. 10
    ろ過filtered
11. 11
    濃縮concentrated under reduced pressure

実験手順

2-methyl-1-phenylpropan-2-yl 2-((4R,6S)-6-((E)-2-(4-(4-fluorophenyl)-6-isopropyl-2-(N-methylmethylsulfonamido)pyrimidin-5-yl)vinyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate (15.38 g) prepared in Example 19 was dissolved in tetrahydrofuran (80 ml) and a 0.1M hydrochloric acid aqueous solution (19.21 ml) was added thereto, followed by stirring for 24 hours while heating to 40° C. The reaction liquid was cooled to room temperature and a 0.5M sodium hydroxide aqueous solution (81 ml) was added thereto over 5 minutes, followed by stirring for 4 hours. Ethyl acetate (250 ml) and purified water (250 ml) were added to the reaction liquid, and the organic layer was separated, washed with saturated sodium chloride (150 ml), dried over anhydrous sodium sulfate, filtered, and then concentrated under reduced pressure to give (E)-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl](3R,5S)-3,5-dihydroxyhept-6-enoic acid sodium salt.

出典