تفاعل #1332467

ord-a6a46054166e47f188ff562b861fc636

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزconcentrated
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in CH2Cl2
  3. 3
    غسيلwashed with water
  4. 4
    استخلاصextracted with 0.5 M HCl
  5. 5
    workup.ADDITIONAfter addition of NaOH and extraction with CH2Cl2 the organic layer
  6. 6
    تجفيفwas dried (Na2SO4)
  7. 7
    أخرىevaporated

الإجراء التجريبي

4-Bromomethyl-3-(4-chlorophenyl)-2-thia-1-azaspiro[4.5]dec-3-ene 2,2-dioxide, made as described in Example 2, (270 mg, 0.69 mmol) was dissolved in ethanol (30 mL). Methylamine (70% solution in water, 8 mL) was added and the mixture was stirred overnight at room temperature and concentrated. The residue was dissolved in CH2Cl2, washed with water and extracted with 0.5 M HCl. After addition of NaOH and extraction with CH2Cl2 the organic layer was dried (Na2SO4) and evaporated to yield 80 mg (34%) of 3-(4-Chlorophenyl)-4-methylaminomethyl-2-thia-1-azaspiro[4.5]dec-3-ene 2,2-dioxide as a solid. MS (IS): 341 [MH]+

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07125840B2uspto-grants-2006_10