反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 6-chloro-4-methyl-8-nitro-9H-β-carboline (80 mg, 0.31 mmol) in MeOH (10 ml) was stirred at RT. Platinum (10% wt. on carbon, 24 mg) catalyst was added thereto and the reaction vessel was capped and vacuum purged 3 times with argon, followed similarly by hydrogen. The reaction mixture was stirred 1.5 hr under 1 atm hydrogen, then vacuum purged with argon, diluted with DCM (10 ml) and filtered through a 0.2 μM syringe filter. The filtrate was concentrated to yield 6-chloro-4-methyl-9H-β-carbolin-8-ylamine (67 mg) as a light brown oil. 1H-NMR (300 MHz, DMSO-d6): δ 9.04 (s, 1); 8.29 (s, 1); 7.74 (d, 1); 7.10 (d, 1); 2.98 (s, 3). NH4OAc standard conditions. DAD Rf=1.89 min. M+H=231.
WORKUP
后处理
- customthe reaction vessel was capped
- customvacuum purged 3 times with argon
- customvacuum purged with argon
- additiondiluted with DCM (10 ml)
- filtrationfiltered through a 0.2 μM syringe
- filtrationfilter
- concentrationThe filtrate was concentrated