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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
THF (1.5 mL), Pd(OAc)2 (20 mg, 0.089 mmol, 8% eq) and 1,2-bis(diphenylphosphino)ethane (35.5 mg, 16% eq) were mixed under N2, degassed and stirred to give orange yellow mixture. A premixed solution of (3-trimethylsilanylallyl)-carbamic acid tert-butyl ester (250 mg, 1.09 mmol) from (7b) and 4-(4-iodo-phenoxymethyl)-2-methyl-quinoline (410 mg, 1.0 eq) from (7c) in benzene (3 ml) was added. The resulting mixture was heated at 50° C. over the weekend, then cooled to rt, diluted with ether, washed with water, dried and concentrated. {2-[4-(2-Methyl-quinolin-4-ylmethoxy)-phenyl]-allyl}-carbamic acid tert-butyl ester (65 mg, 14.8%) was obtained after the crude was purified by flash column chromatography (20%–40% ethyl acetate-hexanes). MS Found: (M+H)+=405.
WORKUP
后处理
- customdegassed
- customto give orange yellow mixture
- temperaturecooled to rt
- washwashed with water
- customdried
- concentrationconcentrated