تفاعل #49818

ord-5c250430b529499aa12d2ccbd03a77bb

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated at 160° C.-170° C. overnight
  2. 2
    درجة الحرارةThe resulting yellow solution was cooled
  3. 3
    أخرىA yellow precipitate was collected
  4. 4
    غسيلwashed with water, and air
  5. 5
    أخرىdried

الإجراء التجريبي

One hundred thirty mg (0.5 mM) of 6-cyanobenzothieno[3,2-h]isoquinoline (4), prepared in Example 1, was suspended in a hot solution of 168 mg (3 mM) KOH in 1 ml glycerine. The reaction mixture was stirred and heated at 160° C.-170° C. overnight. The resulting yellow solution was cooled, diluted with water and made slightly acidic with glacial acetic acid. A yellow precipitate was collected, washed with water, and air dried to yield 120 mg of product. This initial product was recrystallized from a mixture of DMSO and water to give 78 mg product, mp greater than about 305° C. This then was dried at 80° C./0.2 mm overnight, and characterized as compound 6 using I.R. and mass spectrometry.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05424315uspto-grants-1995_06