Chloral → alpha-Trichloromethyl-2-thiophenemethanol

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.

1. temperatureThe solution was heated
2. temperatureunder reflux for 3.5 hr
3. temperatureAfter cooling
4. concentrationthe n-heptane solution was concentrated
5. distillationthe residue was purified by distillation

ORDレコード

ord-28b3a49b4b8d4b40a1cbd8ddf9546e9f

出典データセット

uspto-grants-1980_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04221915