HRID1061337
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
N-{4-[4-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-phenylsulfamoyl]-phenyl}-acetamide (which was obtained in Example 215) (2.2 g, 5.1 mmol) was treated with concentrated hydrochloric acid (50 mL) at 0° C. and then allowed to warm to room temperature. After 30 min., 20 mL of 5 N NaOH was added dropwise and the precipitate was collected by filtration, and dried over P2O5 to give the title compound as a white solid (1.2 g); 1H NMR (300 MHz, DMSO-d6) δ 2.06 (s, 3H), 2.43 (t, J=5.8 Hz, 4H), 3.53 (t, J=5.8 Hz, 4H), 6.85-7.05 (m, 4H), 7.62 (d, J=9.0 Hz, 2H), 7.71 (d, J=9.0 Hz, 2H), 9.81 (s, 1H), 10.35 (s, 1H); MS (ES) m/z: 388.3 (MH+); HRMS Calcd. for C19H21N3O4S(M+):387.1253. Found: 387.1272.
WORKUP
后处理
- filtrationthe precipitate was collected by filtration
- dry with materialdried over P2O5