反应详情

温度

-5 °C

To a mixture of water (25 mL) and TBME (40 mL), dipotassium hydrogen phosphate (45.2 g), tetrabutylammonium hydrogen sulfate (1.76 g), and 3-methoxy-2,2-dimethylpropionic acid [CAS No. 64241-78-7] (6.86 g) were sequentially added. After cooling the resulting mixture to −5° C., a mixture of chloromethyl chlorosulfate (12.8 g) and TBME (10 mL) was added dropwise thereto, and the resulting mixture was stirred overnight at room temperature. Water (50 mL) and TBME (30 mL) were added to the resulting mixture. After shaking the resulting mixture, the organic layer was collected, and TBME (50 mL) was added to the remaining aqueous layer. The resulting mixture was shaken again and the organic layer was collected. The combined organic layers were washed twice with water (30 mL) and with saturated aqueous sodium chloride solution (30 mL), and dried over anhydrous magnesium sulfate. The resulting mixture was filtered, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was distilled (boiling point: 85-86° C./20 mmHg) under reduced pressure to obtain the captioned compound (5.68 g).

1. addition64241-78-7] (6.86 g) were sequentially added
2. additionwas added dropwise
3. stirringAfter shaking the resulting mixture
4. customthe organic layer was collected
5. additionTBME (50 mL) was added to the remaining aqueous layer
6. stirringThe resulting mixture was shaken again
7. customthe organic layer was collected
8. washThe combined organic layers were washed twice with water (30 mL) and with saturated aqueous sodium chloride solution (30 mL)
9. dry with materialdried over anhydrous magnesium sulfate
10. filtrationThe resulting mixture was filtered
11. customthe filtrate obtained
12. concentrationwas concentrated under reduced pressure
13. customThe residue obtained
14. distillationwas distilled (boiling point: 85-86° C./20 mmHg) under reduced pressure