تفاعل #66110

ord-c6b6cd300ebe4d5bb2b195e5a8862289

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated
  2. 2
    درجة الحرارةat reflux for 2 h
  3. 3
    ترشيحInorganic salts were filtered off
  4. 4
    غسيلwashed with acetone (20 mL)
  5. 5
    تركيزThe combined filtrate and washings were concentrated in vacuo
  6. 6
    workup.DISSOLUTIONthe resulting residue then being dissolved in ethyl acetate (25 mL)
  7. 7
    غسيلwashed successively with water (2×20 mL), brine (20 mL)
  8. 8
    تجفيفdried over anhydrous sodium sulfate
  9. 9
    تركيزconcentrated in vacuo

الإجراء التجريبي

Benzyl bromide (0.6 mL, 5.04 mmol) was added dropwise to a mixture of 2-chloro-5-nitro-phenol (800 mg, 4.61 mmol) and potassium carbonate (1.27 g, 9.22 mmol) in acetone (20 mL) at room temperature and heated at reflux for 2 h. Inorganic salts were filtered off and washed with acetone (20 mL). The combined filtrate and washings were concentrated in vacuo, the resulting residue then being dissolved in ethyl acetate (25 mL) and washed successively with water (2×20 mL), brine (20 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to yield 2-benzyloxy-1-chloro-4-nitro-benzene (1.20 g, 99%) as a cream solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524705B2uspto-grants-2013_09