反应详情

Combine p-methoxybenzylmercaptan (0.08 mL, 0.57 mmol) and-sodium hydride (17 mg, 60% oil dispersion, 0.42 mmol) in degassed dimethylformamide (3 mL). After 1 hour, tetra-n-butylammonium iodide (about 5 mg) and 2-(4-(2-bromo-6-phthalimidohexanoyl-amino)-3-oxo-1,3,4,5-tetrahydro-benzo[c]azepin-2-yl)-4-methyl-valeric acid t-butyl ester (0.27 mmol). After 20 hours, quench be the addition of a saturated aqueous ammonium chloride solution and dilute with water (about 5 mL). Extract with ethyl acetate (about 75 mL). Separate the layers and extract the orgainc layer with brine, dry over Na2SO4, filter, and evaporate in vacuo to give the title compound.

1. waitAfter 20 hours
2. customquench
3. additionthe addition of a saturated aqueous ammonium chloride solution
4. additiondilute with water (about 5 mL)
5. extractionExtract with ethyl acetate (about 75 mL)
6. customSeparate the layers
7. extractionextract the orgainc layer with brine
8. dry with materialdry over Na2SO4
9. filtrationfilter
10. customevaporate in vacuo