反应详情

温度

0 °C

Ethyl alcohol (0.63 mL, 10.8 mmol), 2-benzothiazolethiol (2.0 g, 11.9 mmol) and triphenylphosphine (3.1 g, 11.9 mmol) were dissolved in tetrahydrofuran (50 mL) and cooled to 0° C. Then added diisopropylazadicarboxylate (2.3 mL, 11.9 mmol) and continued stirring for 1 hr. Upon completion, the reaction mixture was dried in vacuo, filtered through a plug of silica with 5% ethyl acetate in hexane and dried in vacuo again to yield 2-(ethylthio)-1,3-benzothiazole (2.2 g, HPLC RT=3.05 min.). LC-MS m/z=196.

1. additionThen added diisopropylazadicarboxylate (2.3 mL, 11.9 mmol)
2. customUpon completion, the reaction mixture was dried in vacuo
3. filtrationfiltered through a plug of silica with 5% ethyl acetate in hexane
4. customdried in vacuo again