反应详情

To a solution of 17-ethyl-1,14-dihydroxy-12-[2'-(4"-amino-3"-methoxycyclohexyl)-1'-methylvinyl]-23,25-dimethoxy-13,19,21,27-tetramethyl-11,28-dioxa-4-azatricyclo[22.3.1.04,9 ]octacos-18-ene-2,3,10,16-tetraone in (100 mg) in dry methylene chloride (4 ml) was added 100 mg of freshly prepared BOC-L-glycine anhydride under nitrogen. After stirring at room temperature for 1.5 hours, the reaction mixture was subjected to work-up and the residue was purified on silica gel (5% MeOH/CH2Cl2) to give the 65 mg of BOC protected compound. This material (48 mg) was dissolved in 1 ml of trifluoroacetic acid at -10° and stirred at this temperature. After 30 minutes, the reaction mixture was cooled to -78° and freeze-dried to give the yellow solid. Purification of the crude material by preparative tlc on silica gel (1% NH4OH in 5% MeOH/CH2Cl2) gave 28 mg of the title compound.

1. customthe residue was purified on silica gel (5% MeOH/CH2Cl2)
2. customto give the 65 mg of BOC protected compound
3. stirringstirred at this temperature
4. waitAfter 30 minutes
5. temperaturethe reaction mixture was cooled to -78°
6. customfreeze-dried
7. customto give the yellow solid
8. customPurification of the crude material by preparative tlc on silica gel (1% NH4OH in 5% MeOH/CH2Cl2)