反应详情

温度

0 °C

To a stirred ice cold solution of 3-azido-3-methylbutanoyl chloride (8.00 g, 49.5 mmol) in anhydrous DCE (160 mL) was added diethylamine (15.4 mL, 3 equiv, 0.148 mol) in one portion. The reaction was left to stir at 0° C. for 1 h. Water (200 mL) was added to the reaction mixture and the contents poured into a separatory funnel. The organic layer was separated and washed with water (3×100 mL) and brine (100 mL). It was dried over anhydrous MgSO4, filtered, concentrated and dried under high vacuum to give a crude oil (9.80 g, quant). This material was used without further purification.

1. waitThe reaction was left
2. additionthe contents poured into a separatory funnel
3. customThe organic layer was separated
4. washwashed with water (3×100 mL) and brine (100 mL)
5. dry with materialIt was dried over anhydrous MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customdried under high vacuum
9. customto give a crude oil (9.80 g, quant)
10. customThis material was used without further purification