反应详情

To an ice-cold solution of the diamine of Step A (3.4 g) and triethylamine (4.0 mL) in dry chloroform (50 mL) was added thiophosgene (1.7 mL). After 20 minutes at ambient temperature, the reaction was quenched with water and extracted with dichloromethane. The extracts were combined, dried over sodium sulfate and concentrated in vacuo to give a brown oil. The crude material was dissolved in dichloromethane and absorbed onto a column of Merck-60 flash silica gel. Elution with 11% ethyl acetate in hexane provided an orange solid which was triturated with diethyl ether to give the title product (2.4 g, 59.5%) as a white solid, m.p. 88-90° C.

1. customthe reaction was quenched with water
2. extractionextracted with dichloromethane
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customto give a brown oil
6. customabsorbed onto a column of Merck-60 flash silica gel
7. washElution with 11% ethyl acetate in hexane
8. customprovided an orange solid which
9. customwas triturated with diethyl ether