Chloral → alpha-Trichloromethyl-2-thiophenemethanol
Reaction equation
[S:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[Cl:6][C:7]([Cl:11])([Cl:10])[CH:8]=[O:9]>CCCCCCC>[Cl:6][C:7]([Cl:11])([Cl:10])[CH:8]([C:2]1[S:1][CH:5]=[CH:4][CH:3]=1)[OH:9]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
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.
Workup
- temperatureThe solution was heated
- temperatureunder reflux for 3.5 hr
- temperatureAfter cooling
- concentrationthe n-heptane solution was concentrated
- distillationthe residue was purified by distillation
Sources & evidence
- ORD record
- ord-28b3a49b4b8d4b40a1cbd8ddf9546e9f
- Source dataset
- uspto-grants-1980_09
- Patent number
- US04221915
Reaction notes
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