반응 #55869

ord-28b3a49b4b8d4b40a1cbd8ddf9546e9f

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The solution was heated
  2. 2
    온도under reflux for 3.5 hr
  3. 3
    온도After cooling
  4. 4
    농축the n-heptane solution was concentrated
  5. 5
    workup.DISTILLATIONthe residue was purified by distillation

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04221915uspto-grants-1980_09