تفاعل #816436

ord-47625a4f4d8f4d60b938103a341d55db

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةit was then cooled in an ice-bath
  2. 2
    أخرىThe cooling-bath was removed
  3. 3
    workup.ADDITIONafter the addition
  4. 4
    أخرىevaporated to dryness
  5. 5
    workup.ADDITIONDCM (50 mL) was added to the residue
  6. 6
    غسيلIt was washed with HCl (5%, 10 mL), water (30 mL×3) and brine (20 mL)
  7. 7
    تجفيفdried (MgSO4)
  8. 8
    أخرىevaporated

الإجراء التجريبي

n-Butylamine (3.25 g, 44.43 mmol) was dissolved in THF (25 mL) and it was then cooled in an ice-bath. ((4-Chlorophenyl)methyl)sulfonyl chloride (5.0 g, 22.21 mmol) in THF (25 mL) was dropped in. The cooling-bath was removed after the addition. The mixture was stirred for 2 h and then evaporated to dryness. DCM (50 mL) was added to the residue. It was washed with HCl (5%, 10 mL), water (30 mL×3) and brine (20 mL), dried (MgSO4) and evaporated to give the title compound (5.43 g, 93%) as a solid; 1H NMR (400 MHz, CDCl3): δ 7.36 (d, 2H), 7.32 (d, 2H), 4.19 (s, 2H), 4.11 (bt, 1H), 2.99 (dd, 2H), 1.50-1.43 (m, 2H), 1.36-1.26 (m, 2H), 0.90 (t, 3H); Mass Spectrum: M−H+ 260.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07582629B2uspto-grants-2009_09