4-Hydroxy-3-nitrobenzotrifluoride synthesis
- Product Name:4-Hydroxy-3-nitrobenzotrifluoride
- CAS Number:400-99-7
- Molecular formula:C7H4F3NO3
- Molecular Weight:207.11
Yield: 91%
Reaction Conditions:
with sodium hydroxide in hydrogenchloride;methanol
Steps:
1 EXAMPLE 1
EXAMPLE 1 400 ml of methanol, 20 g of benzyldimethyldodecylammonium chloride and 180 g of 4-chloro-3-nitro-benzotrifluoride are initially introduced into the reaction flask, whilst stirring, and 400 g of 50% strength sodium hydroxide solution are then added dropwise. The temperature rises to about 70° C. if the addition is carried out in the course of about 20 minutes. The mixture is then stirred at 65° C. for a further 4 hours and subsequently cooled by adding ice, and the pH is adjusted to 3 with concentrated hydrochloric acid. The phenol is driven over with steam and the phases are separated in the receiver by adding about 50 ml of concentrated hydrochloric acid. 156 g of 2-nitro-4-trifluoromethylphenol are obtained with a purity of more than 98.5%, according to analysis by gas chromatography, which corresponds to a yield of 91% of theory. Boiling point: 92°-95° C. at 15 mm, nD20: 1.5020.
References:
Bayer Aktiengesellschaft US4225731, 1980, A
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