Table 1.
Optimization of glycosidations of SInMe donor 2 and SInAll donor 6 with 6-OH acceptor 13.
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Entry | Conditions [equiv.] | Yield of 14 |
1 | 2, NIS (3.0), TfOH (0.8), rt, 19 h | 60% |
2 | 2 , NIS (4.0), TfOH (1.0), rt, 15 min | 75% |
3 | 2, NIS (4.5), TMSOTf (1.0), rt, 10 min | 83% |
4 | 2, Ag2CO3 (0.8), TMSOTf (4.0), rt, 3.5 h | 70% |
5 | 6, NIS (2.0), TMSOTf (0.2), rt,16 h | 29% |
6 | 6, NIS (3.0), TMSOTf (0.8), rt, 2 h | 68% |
7 | 6, NIS (3.0), TMSOTf (1.0), rt, 1 h | 89% |
8 | 6, NIS (3.0), TfOH (0.4), rt, 24 h | 52% |
9 | 6, NIS (3.0), TfOH (0.8), rt, 24 h | 69% |
10 | 6, NIS (3.0), TfOH (1.0), rt, 24 h | 73% |
11 | 6 , NIS (3.2), TfOH (1.0), rt, 1 h | 94% |
12 | 6, Ag2CO3 (1.0), TMSOTf (4.0), rt, 1 h | 79% |