反应详情

To N-tert-Butyloxycarbonyl-3-hydroxymethyl-1,2,3,4-tetrahydroisoquinoline (9 g) dissolved in tetrahydrofuran (200 mL) at 0° C. was added sodium hydride (60% in mineral oil 1.64 g). The mixture wa stirred for 50 minutes then, carbon disulfide (2.5 mL) was added and stirred for an additional 1 hour. Then methyl iodide (2.55 mL) was added and after two hours ammonium hydroxide (28% solution, 10.4 mL) was added. After overnight stirring, brine was added, the mixture was extracted with methylene chloride and the extract concentrated to yield the product as a solid (5.6 g).

1. stirringstirred for an additional 1 hour
2. additionwas added
3. stirringAfter overnight stirring
4. extractionthe mixture was extracted with methylene chloride
5. concentrationthe extract concentrated