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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 1 M 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 2 M 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