preparation | the preparation of 1-tert-butyl oxycarbonamide cyclohexarboxylic acid is as follows: sodium hydroxide solution (43mL,4mol/L), THF(40mL) and 1-aminocyclohexanoic acid (5.0g,34.96mmol) are added to the round bottom flask, and ditert-butyl dicarbonate (9.13g,41.96mmol), after dropping, the reaction system was stirred overnight at room temperature. Water (100mL) was added to the reaction system, acidified with hydrochloric acid (50mL,1mol/L), then extracted with ethyl acetate (50mL × 2), and organic phases were combined. The organic phases were washed with saturated salt water (100mL × 2) and anhydrous sodium sulfate was dried. Filtration, vacuum evaporation to remove the solvent, crude product by silica gel column chromatography purification (petroleum ether/ethyl acetate (V/V)= 4/1), to obtain a white solid title compound 1-tert-butyl oxycarbonamide cyclohexanocarboxylic acid (7.3g,86%). |
hazardous treatment | if 1-tert-butyloxy carboxylic acid is inhaled, please move the patient to fresh air. If the skin is in contact with the skin, remove the contaminated clothes, rinse the skin thoroughly with soapy water and clear water, and see a doctor if you feel uncomfortable. If the eyes are in clear contact, separate the eyelids and rinse with flowing water or normal saline, and seek medical treatment immediately; if ingestion, gargle immediately, forbid vomiting, should seek medical treatment immediately. |