تفاعل #1583866

ord-10ce34f5a57644c6bb2be09881066810

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
-20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter the completion of reaction
  2. 2
    غسيلThe resulting mixture was washed with a saturated aqueous NaCl solution
  3. 3
    تجفيفdried over Na2SO4
  4. 4
    أخرىpurified by column chromatography (silica gel column, eluted with petroleum ether: ethyl acetate=20:1 (volumetric ratio))
  5. 5
    أخرىto produce the product of 1-benzyl-3-methylpyrrolidinyl-3-ol (0.7 g) in a yield of 58.1%

الإجراء التجريبي

1-benzylpyrrolidone (1.1 g, 6.3 mmol) was dissolved in 4 mL THF under stirring at −20° C. The resulting solution was dropwisely added to a solution of methyl magnesium bromide (13.2 mL, 12.2 mmol) in THF. The stirring was continued for 3 hours. After the completion of reaction, the reaction solution was dropwisely added to an ice water. The resulting mixture was washed with a saturated aqueous NaCl solution, dried over Na2SO4, and purified by column chromatography (silica gel column, eluted with petroleum ether: ethyl acetate=20:1 (volumetric ratio)) to produce the product of 1-benzyl-3-methylpyrrolidinyl-3-ol (0.7 g) in a yield of 58.1%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09198902B2uspto-grants-2015_12