HRID83969
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
3-decanyl-6-dec-1-ynyldithieno[3,2-b:2′,3′-d]thiophene (93) (36.0 g, 0.076 mol) is dissolved into ethyl acetate (60 mL), and 5% Pt/C (9.0 g) is added to the solution. The mixture is stirred under a H2 atmosphere (90 psi) for 24 hours and then filtered. After removal of the ethyl acetate, the residue is purified by chromatography on silica gel eluted with hexane to produce the target compound (29.0 g, 79.9% yield). 1HNMR (CD2Cl2): δ 7.29 (d, 1H), 7.27 (d, 1H), 2.80 (t, 2H), 2.67 (t, 2H), 1.68-1.27 (m, 32H), 0.88 (m, 6H). 13CNMR. 142.88, 140.75, 139.82, 131.69, 131.37, 126.69, 125.04, 120.94, 32.16, 29.85 (m, overlap), 22.93, 14.11.
WORKUP
后处理
- additionis added to the solution
- filtrationfiltered
- customAfter removal of the ethyl acetate
- customthe residue is purified by chromatography on silica gel
- washeluted with hexane