تفاعل #163426

ord-2881d6ca74c5407e8f5f4edf29f409b2

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONthrough the addition so an ice bath
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    ترشيحfiltered through celite under a stream of N2
  4. 4
    غسيلwashed with 20 mL dry CH2Cl2
  5. 5
    أخرىThe solvent was evaporated
  6. 6
    أخرىto give a pale yellow liquid

الإجراء التجريبي

To t-butyl amine (5.25 mL, 50.0 mmol) and MgSO4 (2 g) in CH2Cl2 (10 mL) at room temperature was added slowly hexanal (6.0 mL, 50 mmol) under N2 at room temperature. The reaction became exothermic halfway through the addition so an ice bath was briefly used to control the reaction rate and avoid boiling off the solvent or amine. After the addition was complete, the reaction was stirred at room temperature for 2 h, filtered through celite under a stream of N2 and washed with 20 mL dry CH2Cl2. The solvent was evaporated to give a pale yellow liquid. 1H NMR (300 MHz, CDCl3) δ 0.87-0.91 (m, 3H), 1.17 (s, 9H), 1.25-1.35 (m, 4H), 1.45-1.55 (m, 2H), 2.23 (m, 2H), 7.59 (t, 1H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08835475B2uspto-grants-2014_09