反応 #2122515

ord-3247d68618be469cb5d0456968bcc548

反応方程式

O=S(=O)(O)Cl
Chlorosulfonic acid
Cc1nc2ccccc2o1
2-methylbenzoxazole
Cc1nc2ccc(S(=O)(=O)Cl)cc2o1
Compound 8
収率 59.9%
Cc1nc2ccc(S(=O)(=O)Cl)cc2o1
2-methylbenzoxazole-6-sulfonyl chloride
収率 59.9%

反応条件

温度
117.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他of 15 min
  2. 2
    温度After cooling
  3. 3
    workup.ADDITIONmix
  4. 4
    その他The white solid that separated
  5. 5
    ろ過was collected by filtration
  6. 6
    洗浄washed with water until washings
  7. 7
    その他dried

実験手順

Chlorosulfonic acid (12.5 ml, 187.8 mmol) was cooled in an ice bath and 2-methylbenzoxazole (5.0 g, 37.5 mmol) was carefully added drop wise over a period of 15 min. The combined mixture was heated at 115-120° C. for 16 hours. After cooling, the mixture was added very slowly to ca. 100 ml ice/water mix. The white solid that separated was collected by filtration, washed with water until washings were neutral and dried to yield 5.2 g (59%) of Compound 8, whose structure is given below:

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08574881B2uspto-grants-2013_11