تفاعل #1166472

ord-8f88d73a3f4447a087445e19ee915977

معادلة التفاعل

CNCCO
2-(methylamino)ethanol
O=C(Cl)c1ccco1
furoyl chloride
CN(CCO)C(=O)c1ccco1
N-(2-hydroxyethyl)-N-methylfuranamide
المردود 57.6%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىA one liter, three necked flask was equipped with overhead stirrer
  2. 2
    درجة الحرارةThe reaction flask was cooled with an ice bath
  3. 3
    غسيلThe dichloromethane was washed with NaCl(aq.)
  4. 4
    استخلاصNext, the NaCl(aq.) layer was extracted with dichloromethane
  5. 5
    تجفيفdried over MgSO4
  6. 6
    أخرىThe dichloromethane was removed with a rotoevaporator

الإجراء التجريبي

A one liter, three necked flask was equipped with overhead stirrer, nitrogen atmosphere and an addition funnel. The flask was charged with 115 g of 2-(methylamino)ethanol (1.53 mol.) and 500 ml of dichloromethane. The reaction flask was cooled with an ice bath. Next, 100 g of furoyl chloride (0.77 mol.) was slowly added via the addition funnel over 2.5 hours. The dichloromethane was washed with NaCl(aq.). Next, the NaCl(aq.) layer was extracted with dichloromethane and the two dichloromethane layers were combined and dried over MgSO4. The dichloromethane was removed with a rotoevaporator to yield 75 g (44%) of N-(2-hydroxyethyl)-N-methylfuranamide.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05580647uspto-grants-1996_12