反应详情

To a stirred solution of 1,3-dichloroacetone (5.00 g, 39.37 mmol) in tetrahydrofuran (50 mL) were added 2-t-butyloxycarbonylaminoethanethiol (6.98 g, 37.50 mmol) and triethylamine (3.77 g, 37.50 mmol) at 0° C. After 3 hours the reaction mixture was partitioned between ethyl acetate and water. Organic layer was washed with 1 M hydrochloric acid, water, sodium bicatbonate solution and brine. Organic extract was dried over sodium sulfate and concentrated under reduced pressure to afford oily residue of title product (9.40 g). 1H NMR (CDCl3) δ 1.58 (s, 9H), 2.76 (t, J=6, 2H), 3.40 (m, 2H), 3.58 (s, 2H), 4.42 (s, 2H), 5.00 (br s, 1H).

1. customAfter 3 hours the reaction mixture was partitioned between ethyl acetate and water
2. washOrganic layer was washed with 1 M hydrochloric acid, water, sodium
3. extractionOrganic extract
4. dry with materialwas dried over sodium sulfate
5. concentrationconcentrated under reduced pressure