1-Hydroxybenzotriazole hydrate → HCID 10229408, compound

Participants

Reaction Steps

A solution of the product of Example 4 Step 2 (265 mg, 1.18 mmol) in DMF (5 ml) was treated with N-cyclohexylcarbodiimide, N′-methyl polystyrene (1.8 g) and 1-hydroxybenzotriazole hydrate (162 mg, 1.19 mmol). The mixture was stirred at room temperature for 30 minutes and then treated with a solution of the product of Example 3 Step 2 (407 mg, 1.19 mmol) in DMF (2 ml). After stirring for a further 16 hours, the reaction mixture was applied to a Bond Elut SCX cartridge. The cartridge was eluted with methanol and then 0.880 ammonia solution/methanol (1:9) to elute the product. After concentrating in vacuo, the product was purified further by chromatography on silica gel eluting with chloroform/ethanol/0.880 ammonia solution (90:9:1) to yield the title compound (340 mg, 56%); MS (ES+) m/e 512, 514 [M+H]+.

Provenance & Evidence