تفاعل #86484

ord-fc05b04f677e40c5994d7bc155187ab9

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    استخلاصThe aqueous layer was extracted with ether three times
  3. 3
    تجفيفThe combined organic layer was dried over MgSO4
  4. 4
    أخرىevaporated
  5. 5
    أخرىwas dried under high vacuum

الإجراء التجريبي

2-(methylamino)ethanol (1.0 g, 13.3 mmol) was stirred in DCM (25.0 ml) under atmosphere of nitrogen. DIEA (3.23 ml, 18.6 mmol) followed by tert-butylchlorodimethylsilane (2.0 g, 13.3 mmol) was added and the reaction mixture was stirred at room temperature over night. The reaction mixture was poured into ether/water. The aqueous layer was extracted with ether three times. The combined organic layer was dried over MgSO4 and evaporated and remaining material was dried under high vacuum to afford title compound (1.4 g, yield: 56%). 1H-NMR (400 MHz, CDCl3) δ 0.08 (s, 6H) 0.91 (s, 9H) 1.93 (br. s., 1H) 2.48 (s, 3H) 2.71 (t, 2H) 3.75 (t, 2H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434697B2uspto-grants-2016_09