Ethanol → HCID 21559438, compound

Temperature

-78 °C

A mixture of isobutyraldehyde (0.25 mole), ethanol (0.4 g) and dichloromethane (75 ml) was placed in a three-necked flask fitted with a gas inlet tube, a Dry Ice condenser and a gas outlet tube connected to a gas trap cooled to -78°C. Trifluoromethanesulfenyl chloride (0.22 mole) was added to the cold solution which was maintained under a nitrogen atmosphere. (Caution: It should be noted that trifluoromethanesulfenyl chloride is a highly hazardous material which must be handled with care to avoid inhalation or contact with the skin.) The reaction mixture was then allowed to warm to about 25°C and stirred magnetically until the orange colored solution had become nearly colorless (about 6 hours). The reaction mixture was then distilled. The distillation assembly was connected to a -78°C gas trap to trap any unreacted trifluoromethylsulfenyl chloride. The 2-trifluoromethylthio-2-methylpropionaldehyde, b.p. 108°-116°C was identified by spectral and elemental analyses of a purified sample, b.p. 116°C.

1. customwas placed in a three-necked flask
2. customfitted with a gas inlet tube, a Dry Ice condenser and a gas outlet tube
3. customconnected to a gas trap
4. temperaturewas maintained under a nitrogen atmosphere
5. temperatureto warm to about 25°C
6. custom(about 6 hours)
7. distillationThe reaction mixture was then distilled
8. distillationThe distillation
9. customassembly was connected to a -78°C

ORD record

ord-72c10ed24fea47b58481d8a4ebf47829

Source dataset

uspto-grants-1976_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03937738