تفاعل #67680

معادلة التفاعل

2-methyl-1-phenylpropan-2-yl 2-((4R,6S)-6-(chloromethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate

sodium 1-phenyl-1H-tetrazole-5-thiolate

→

title compound

المردود 97.2%

2-methyl-1-phenylpropan-2-yl 2-((4R,6S)-2,2-dimethyl-6-((1-phenyl-1H-tetrazol-5-ylthio)methyl)-1,3-dioxan-4-yl)acetate

المردود 97.2%

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction liquid
2. 2
   أخرىThe reaction liquid
3. 3
   درجة الحرارةwas cooled to room temperature
4. 4
   أخرىdiisopropyl ether (600 ml) and purified water (600 ml)
5. 5
   workup.ADDITIONwere added
6. 6
   أخرىThe organic layer was separated
7. 7
   غسيلwashed with purified water (600 ml)
8. 8
   تجفيفa 10% sodium bicarbonate aqueous solution (600 ml), a saturated ammonium chloride aqueous solution (600 ml) and a saturated sodium chloride aqueous solution (600 ml), dried over anhydrous magnesium sulfate
9. 9
   ترشيحfiltered
10. 10
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

2-methyl-1-phenylpropan-2-yl 2-((4R,6S)-6-(chloromethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate (30 g) prepared in Example 5 was dissolved in dimethylformamide (150 ml), and sodium 1-phenyl-1H-tetrazole-5-thiolate (33.9 g) prepared in Example 7 was added thereto. The reaction liquid was warmed to 90° C. and then stirred for 24 hours. The reaction liquid was cooled to room temperature, and diisopropyl ether (600 ml) and purified water (600 ml) were added thereto. The organic layer was separated, washed with purified water (600 ml), a 10% sodium bicarbonate aqueous solution (600 ml), a saturated ammonium chloride aqueous solution (600 ml) and a saturated sodium chloride aqueous solution (600 ml), dried over anhydrous magnesium sulfate, filtered, and then concentrated under reduced pressure to give the title compound (40.8 g).

المصدر