background and overview[1]
2,3-dichlorobenzamide can be used as a pharmaceutical synthesis intermediate. if 2,3-dichlorobenzamide is inhaled, move the patient to fresh air; if the skin comes into contact, take off contaminated clothing, rinse the skin thoroughly with soap and water, and seek medical attention if you feel uncomfortable; if the eyes if exposed to sunlight, separate eyelids, rinse with running water or saline, and seek medical attention immediately; if ingested, rinse mouth immediately, do not induce vomiting, and seek medical attention immediately.
structure
preparation[1]
the preparation of 2,3-dichlorobenzamide is as follows: add 2,3-dichlorobenzoic acid (10.0g, 52.4mmol) and ethanol solution to 100ml toluene, add oxalyl chloride (7.0g, 55mmol) and heat to reflux 4 hours, cooled and concentrated. the resulting acid chloride was added to a mixture of etoac and 12n ammonium and stirred vigorously. the brine etoac layer was washed with 1 m hcl, dried (mgso4), and concentrated to obtain 9.4 g of 2,3-dichlorobenzamide. 1hnmr (cdcl3) 6.06.06 (bs, 2h), 7.28 (t, j) 8hz, 1h), 7.54-7.62 (m, 2h). ms(dci/nh3)m/e207(m+nh4)+.
apply[1]
2,3-dichlorobenzamide can be used as a pharmaceutical synthesis intermediate. for example, to prepare 2,3-dichlorobenzonitrile, the specific steps are as follows: 2,3-dichlorobenzamide (9.4g, 50mmol) (150ml) in pocl3 is heated at 95℃ for 2 hour. the solution was cooled and concentrated. dissolve the residue in etoac and separate. add 10% k2co3 aqueous solution to the aqueous layer. wash the etoac layer with brine (2 × 50 ml), dry (mgso4), and concentrate to obtain 8.2g 2,3-dichlorobenzonitrile, melting point 60-61℃. 1hnmr (cdcl3)ä7.34 (t, j) 8hz, 1h), 7.62 (dd, j) 8.1hz, 1h), 7.71 (dd, j) 8.1hz, 1h).
main reference materials
[1]structure-activitystudiesforanovelseriesoftricyclicsubstituted hexahydrobenz[e]isoindoler1aadrenoceptorantagonistsaspotentialagentsforthesymptomatictreatmentofbenignprostatichyperplasia(bph)
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