反应详情

To a 5 L hydrogenator was charged the product from step (viii) above (209.4 g, 0.693 mol), methanol (1675 mL, 8 volumes) and 10% Pd/C (10.2 g). The vessel was purged with 3×N2 and 3×H2 and then stirred under 0.3447 MPa (50 psi) H2 until no further exotherm was observed, with HPLC indicating 96.35% product and 1.10% starting material. The reaction was diluted with THF (314 mL) and the catalyst was removed via vacuum filtration (Cuno filter), before being washed with THF (1000 mL). The solvents were concentrated to isolate a light brown solid, which was dried under vacuum at 40° C. overnight. Yield=167.0 g (88.5%). HPLC purity 96.7%. Purity >95% by 1H NMR.

1. customThe vessel was purged with 3×N2 and 3×H2
2. additionThe reaction was diluted with THF (314 mL)
3. customthe catalyst was removed via vacuum filtration (Cuno filter)
4. washbefore being washed with THF (1000 mL)
5. concentrationThe solvents were concentrated
6. customto isolate a light brown solid, which
7. customwas dried under vacuum at 40° C. overnight