preparation method of 1-(3,5-dichlorophenyl)piperazine_kain industrial additive

background and overview^[1]

1-(3,5-dichlorophenyl)piperazine can be used as a pharmaceutical synthesis intermediate. if 1-(3,5-dichlorophenyl)piperazine is inhaled, move the patient to fresh air; if skin contact occurs, remove contaminated clothing and rinse skin thoroughly with soap and water. if discomfort occurs , seek medical attention; if eye contact occurs, 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.

preparation^[1]

1-(3,5-dichlorophenyl)piperazine can be used as a pharmaceutical synthesis intermediate, such as the preparation of compound 2-(((4-(3,5-dichlorophenyl)piperazine-1- (bromoacetyl)amino)-6-methoxybenzothiazole, the specific steps are as follows: 2-((bromoacetyl)amino)-6-methoxybenzothiazole (1.0g, 3.32mmol), 1- (3,5-dichlorophenyl)piperazine (1.0g, 4.40mmol) and anhydrous k2co3 (0.61g, 4.40mmol) were dissolved in dmf (30ml), and the mixture was poured into ice water (200ml) and washed with etoac (3×50ml) extraction. the organic layer was dried (mgso4), filtered, and the residue was purified by silica gel chromatography, eluting with hexane-ethyl acetate (2:1) to obtain 1.01 g (67%) of the title compound 2-(((4-(3) , 5-dichlorophenyl)piperazin-1-yl)acetyl)amino)-6-methoxybenzothiazole, solid, melting point 80-81°c:

1hnmr (dmso-dg) δ12.03 (bs, 1h), 7.63 (d, j=9.2, 1h), 7.57 (d, j=2.4, 1h), 7.03 (dd, j=8.8, j= 2.4, 1h), 6.94 (d, j=1.6, 2h), 6.85 (t, j=1.6, 1h), 3.81 (s, 3h), 3.39 (s, 2h), 3.27 (t, j=4.8, 4h ), 2.65 (t, j=4.8, 4h);

13cnmr (dmso-d6) δ168.97, 156.15, 155.43, 152.59, 142.52, 134.61, 132.74, 121.12, 116.93, 114.92, 113.02 (2c), 104.72, 59.91, 55.59, 52.05 (2 c), 47.14.

main reference materials

[1] wo1999031096 piperazine derivatives useful as hypoglycemic agents