تفاعل #55869

ord-28b3a49b4b8d4b40a1cbd8ddf9546e9f

معادلة التفاعل

c1ccsc1
Thiophene
O=CC(Cl)(Cl)Cl
trichloroacetaldehyde
OC(c1cccs1)C(Cl)(Cl)Cl
α-trichloromethyl-2-thiophenemethanol
المردود 20.0%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe solution was heated
  2. 2
    درجة الحرارةunder reflux for 3.5 hr
  3. 3
    درجة الحرارةAfter cooling
  4. 4
    تركيزthe n-heptane solution was concentrated
  5. 5
    workup.DISTILLATIONthe residue was purified by distillation

الإجراء التجريبي

Thiophene (4.2 g, 50 mmol) and trichloroacetaldehyde (7.35 g, 50 mmol) were dissolved in n-heptane (25 ml). The solution was heated under reflux for 3.5 hr. under a Soxleht apparatus in which Amberlyst 15 (4.2 g) had been placed. After cooling, the n-heptane solution was concentrated, and the residue was purified by distillation to give 2.32 g of α-trichloromethyl-2-thiophenemethanol boiling at 98°-100° C./1.0 mmHg.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04221915uspto-grants-1980_09