HRID1468229
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
HCl (4 M in 1,4-dioxane) (8.38 mL, 33.5 mmol) was added to a warm solution of N-(7′-bromo-3′,4′-dihydro-1′H-spiro[cyclopropane-1,2′-naphthalene]-1′-ylidene)-2-methylpropane-2-sulfinamide (Intermediate 10, 1.19 g, 3.35 mmol) in dry dioxane (12 mL) under Ar (g). The mixture was stirred at r.t. for 40 min after which diethyl ether was added. The precipitate was filtered and washed with diethyl ether and then taken up in CH2Cl2 and washed twice with sat. aq. NaHCO3. The organic phase was dried (Na2SO4), filtered and concentrated to give the title compound (0.717 g, 85% yield). MS (ES+) m/z 250.0 [M+H]+.
WORKUP
后处理
- additionwas added
- filtrationThe precipitate was filtered
- washwashed with diethyl ether
- washwashed twice with sat. aq. NaHCO3
- dry with materialThe organic phase was dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated