反应详情

A solution of 1,3,4,9-tetrahydro-beta-carboline-1,2-dicarboxylic acid 2-benzyl ester (3.7 mg, 9.4 mmol) in THF (100 ml) under N2 was cooled to −78° C. 1.5M DIBAL in toluene solution (31.2 ml, 47 mmol) was added over 2 hours. After stirring for 4 hours the reaction mixture was quenched with methanol and water, extracted into EtOAc and washed with dilute aqueous HCl. The organic layer was dried over Na2SO4, filtered and evaporated to dryness. LCMS purity 50%, m/z 335 [M++H]+ The material was used in the next stage without further purification.

1. customwas quenched with methanol and water
2. extractionextracted into EtOAc
3. washwashed with dilute aqueous HCl
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. customevaporated to dryness
7. customLCMS purity 50%, m/z 335 [M++H]+ The material was used in the next stage without further purification