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With sodium tetrahydroborate; In ethanol; at 0 - 20℃; for 16.5h;
b) (4-Methanesulfonyl-2-trifluoromethyl-phenyl)-methanol:; To a suspension of 4-methanesulfonyl-2-trifluoromethyl-benzaldehyde (49.2 g, 0.20 mol) in dry EtOH (500 ml), cooled in an ice-bath, is added sodium borohydride (10.8 g, 0.22 mol), portionwise over 30 mins. The reaction mixture is allowed to warm up slowly to room temperature then stirring is continued for 16 h. The reaction mixture is poured into a beaker of crushed ice (700 ml) and adjusted to pH 1 with 2N HCI (approx. 200 ml). The resulting pale yellow suspension is extracted with CH2CI2 (3 x 150 ml), dried (MgSO4) and evaporated to dryness in vacuo, to afford a pale yellow solid.
10 g
With methanol; sodium tetrahydroborate; at 0 - 20℃; for 2.0h;
Charged 10. Og of <strong>[1215310-75-0]4-(methylsulfonyl)-2-(trifluoromethyl)benzaldehyde</strong> in methanol and added 1.5 eq of sodium borohydride at 0C. Heated the reaction to room temperature and stirred for 2hrs. After completion of reaction, quenched the reaction with water and extracted the compound in ethyl acetate (3x). Combined the organic layers and concentrated under vacuum to give 10. Og of (4-(methyl sulfonyl)-2-(trifluoromethyl)phenyl)methanol.
4-(methanesulfonyl)-2-(trifluoromethyl)benzaldehyde oxime[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
97.4%
With hydroxylamine hydrochloride; In ethanol; water; at 20 - 35℃; for 2.5h;
. Compound CI (277g) and 95%EtOH (1320g) were charged into the reactor at 20~30C. Then the mixture was stirred for 0.5h at 20~30C.2. While maintaining the temperature at 20-30C, a solution of Hydroxy lamine hydrochloride (91.5g) in water (23 Og) was added into the mixture.3. The mixture was heated to 25-35C for reaction. After 2h, the mixture was sampled to be analyzed by TLC.4. The mixture was evaporated to remove ethanol, and then water (lOOOg) was charged into the reactor. 5. The mixture was cooled to 5-10C, and 10% NaOH solution (630g) was added dropwise at 10C~20C to adjust pH=8~9.6. The mixture was filtered with a nutsche filter. The filter cake was rinsed with water (lOOOg).7. The filter cake was dried at 40~45C on vacuum to afford compound C2.Example IResultsExamples 2 and 3: Preparation of C3 (4-(methanesulfonyl)-2-(trifluoromethyl)phenyl) methanamine)