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
Enantiomer C of cis-4-[4-(octahydro-quinoline-1-carbonyl)-thiophen-2-yl]-pipendine-1-carboxylic acid tert-butyl ester [Enantiomer C] (0.06 g, 0.14 mmol) was dissolved in DCM (3 mL) and TFA (3 mL) and the reaction stirred at room temperature for 5 hours. The solvent was evaporated and the residue product was purified by flash chromatography on a SCX-2 cartridge, washing with acetonitrile and then eluting with 2 M ammonia in methanol. The fractions containing the desired product were concentrated under vacuum to give the title compound (0.056 g). LCMS m/z 333.20 [M+H]+ RT=6.44 min (Analytical Method 2). 1H NMR (400 MHz, CHCl3-d): δ 7.2 (s, 1H), 6.9 (s, 1H), 4.6 (m, 1H), 3.8 (m, 1H), 3.2 (m, 2H), 3.1 (m, 1H), 2.9 (m, 1H), 2.7 (m, 2H), 2.0-1.1 (m 18H).
WORKUP
后处理
- customThe solvent was evaporated
- customthe residue product was purified by flash chromatography on a SCX-2 cartridge
- washwashing with acetonitrile
- washeluting with 2 M ammonia in methanol
- additionThe fractions containing the desired product
- concentrationwere concentrated under vacuum