反应 #1747867

ord-3997275d56804cd7b800fc4a35bd29a2

反应方程式

O=S1(=O)c2ccccc2N(c2ccc(OCc3ccccc3)cc2)c2ccccc21
10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide
O=C[O-].[NH4+]
ammonium formate
O=S1(=O)c2ccccc2N(c2ccc(O)cc2)c2ccccc21
10-(4-Hydroxyphenyl)phenothiazine 5,5-dioxide

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the solution was filtered
  2. 2
    浓缩The filtrate was concentrated
  3. 3
    workup.ADDITIONafter adding 10 ml of methanol
  4. 4
    过滤The solid was filtered off with suction
  5. 5
    洗涤washed with methanol
  6. 6
    其他dried at 110° C. in a vacuum
  7. 7
    其他drying cabinet
  8. 8
    其他were obtained

实验过程

3.10 g (7.50 mmol) of 10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide, 2.30 g (35.7 mmol) of 98% ammonium formate and 7.5 g of 10% palladium on activated carbon were heated to boiling under reflux in 225 ml of acetone for 1 hour. After cooling to room temperature, the solution was filtered. The filtrate was concentrated and, after adding 10 ml of methanol, stirred overnight. The solid was filtered off with suction, washed with methanol and dried at 110° C. in a vacuum drying cabinet. 1.47 g (61% of theory) of analytically pure light gray microcrystals having an m.p. of 308-311° C. were obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08029919B2uspto-grants-2011_10