HRID1770986

反应详情

EQUATION

反应方程式

HRID 1770986 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

HCl (4 M in 1,4-dioxane) (3.26 mL, 13.0 mmol) was added to a suspension of N-(5′-bromo-4-(difluoromethyl)spiro[cyclohexane-1,2′-indene]-3′(1′H)-ylidene)-2-methylpropane-2-sulfinamide (Example 128 Step 1, 0.564 g, 1.30 mmol) in 1,4-dioxane (5 mL) and the resulting mixture was stirred under a nitrogen atmosphere at r.t. overnight. The formed precipitate was filtered off and washed with Et2O. The solid was then dissolved in DCM and sat. aq. NaHCO3. The mixture was poured into a phase separator, the organic layer was collected and concentrated to yield the title compound that was used as such in the next step: MS (CI) m/z 328 [M+H]

WORKUP

后处理

  1. filtrationThe formed precipitate was filtered off
  2. washwashed with Et2O
  3. dissolutionThe solid was then dissolved in DCM
  4. additionThe mixture was poured into a phase separator
  5. customthe organic layer was collected
  6. concentrationconcentrated