反应详情

Phosphorus oxychloride (34.4 mg, 0.22 mmol) was added to a solution of [(S)-1-((R)-9-amino-5-naphthalen-1-ylmethyl-4-oxo-2,3,4,5-tetrahydro-benzo[b][1,4]thiazepin-3-ylcarbamoyl)-ethyl]-methyl-carbamic acid tert-butyl ester (80 mg, 0.15 mmol) and 5-oxo-hexanoic acid (29.2 mg, 0.22 mmol) in pyridine (1.0 mL). After 2 h, the mixture was poured into 0.5 M HCl (5 mL) and extracted with EtOAc, the combined extracts were washed with water, brine, dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel chromatography to afford the title compound. HR-MS: calcd. for C30H34N4O4S (MH+) 547.2374. found 547.2374.

1. extractionextracted with EtOAc
2. washthe combined extracts were washed with water, brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by silica gel chromatography