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温度

0 °C

5,9-Bis(benzyloxymethyl)-1-thia-4,7,10-triazacyclododecane-3,11-dione (0.352 g, 0.769 mmol) was dissolved in dry THF (10 ml) and cooled to 0° C. A 1M solution of borohydride -THF complex in THF (5 ml) was added under nitrogen and the mixture was stirred for 1 hour at ambient temperature and refluxed for 0.5 hours. To the cooled solution was added 2M hydrochloric acid (3 ml) and the resulting mixture was evaporated to dryness. Water (1 ml) and 25% ammonia solution (1 ml) was added and the mixture was extracted 3 times with 4 ml chloroform. The combined extracts were concentrated in vacuo and gave a yellow oil which showed absence of carbonyl bands in IR. Yield: 0.29 g (88%), FAB MS: 430(M+1).

1. temperaturerefluxed for 0.5 hours
2. customthe resulting mixture was evaporated to dryness
3. additionWater (1 ml) and 25% ammonia solution (1 ml) was added
4. extractionthe mixture was extracted 3 times with 4 ml chloroform
5. concentrationThe combined extracts were concentrated in vacuo
6. customgave a yellow oil which