تفاعل #66699

ord-a9f5a60f72a54a549e71718d9d7bc936

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwas evaporated under reduced pressure
  2. 2
    أخرىThe residue was partitioned between dichloromethane and saturated aqueous potassium carbonate
  3. 3
    أخرىThe organic layer was separated
  4. 4
    غسيلwashed with water
  5. 5
    تجفيفdried (MgSO4)
  6. 6
    ترشيحfiltered
  7. 7
    أخرىevaporated under reduced pressure

الإجراء التجريبي

To a stirred suspension of 2-(1-Hydroxy-1-methyl-ethyl)-4-methoxy-5-piperazin-1-yl-phenol (0.5 g, 1.9 mmol) in dichloromethane under nitrogen at room temperature was added trifluoroacetic acid (7.2 mL, 93.86 mmol) followed by triethyl silane (3.0 mL, 18.8 mmol). The reaction mixture was stirred for 18 hours at room temperature, and then was evaporated under reduced pressure. The residue was partitioned between dichloromethane and saturated aqueous potassium carbonate. The organic layer was separated, washed with water, dried (MgSO4), filtered, and evaporated under reduced pressure to afford 0.47 g (99%) of 2-Isopropyl-4-methoxy-5-piperazin-1-yl-phenol as an oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524725B2uspto-grants-2013_09