تفاعل #49300

ord-f29d2c55f8e14432ae1c7469bd2ce4d9

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThen, the mixture was extracted with ethyl acetate
  2. 2
    غسيلThe organic layer was washed with saturated brine
  3. 3
    تجفيفdried over anhydrous sodium sulfate
  4. 4
    أخرىThe solvent was evaporated under reduced pressure

الإجراء التجريبي

In a similar manner to Step 2 of Example 6, 4-chloro-7-[1-(tert-butoxycarbonyl)-5-formylindol-2-yl]isoindolinone (30.0 mg, 0.0730 mmol) was dissolved in acetonitrile (2 mL), and the solution was treated with N,N-dimethylamine hydrochloride (120 mg, 1.47 mmol), triethylamine (0.162 mL, 1.17 mmol), acetic acid (0.084 mL, 1.5 mmol) and sodium triacetoxyborohydride (154 mg, 0.727 mmol). The reaction mixture was added with water and ethyl acetate. The mixture was added with sodium carbonate to adjust the pH to 9. Then, the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to obtain 4-chloro-7-[1-(tert-butoxycarbonyl)-5-(dimethylaminomethyl)indol-2-yl]isoindolinone (37.8 mg).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745641B2uspto-grants-2010_06