HRID368389

反应详情

EQUATION

反应方程式

HRID 368389 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,5,6,7-Tetrahydro-s-Hydrindacen-1(2H)-one (12.00 g, 0.06967 moles) was stirred in diethyl ether (200 mL) at 0° C. as PhMgBr (0.105 moles, 35.00 ml, of 3.0 M solution in diethyl ether) was added slowly. This mixture was then allowed to stir overnight at room temperature. After the reaction period the mixture was quenched by pouring over ice. The mixture was then acidified (pH=1) with HCl and stirred vigorously for 2 hours. The organic layer was then separated and washed with H2O (2×100 mL) and then dried over MgSO4. Filtration followed by the removal of the volatiles resulted in the isolation of the desired product as a dark oil (14.68 g, 90.3% yield).

WORKUP

后处理

  1. additionwas added slowly
  2. customAfter the reaction period the mixture
  3. customwas quenched
  4. additionby pouring over ice
  5. stirringstirred vigorously for 2 hours
  6. customThe organic layer was then separated
  7. washwashed with H2O (2×100 mL)
  8. dry with materialdried over MgSO4
  9. filtrationFiltration
  10. customfollowed by the removal of the volatiles