Sulfuric Acid → HCID 14098166, compound
Reaction equation
CN([CH2:4][CH:5]([CH2:18][CH2:19][CH2:20][Cl:21])[C:6]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([Cl:16])[C:9]=1[Cl:17])=[O:7])C.S(=O)(=O)(O)O>>[Cl:21][CH2:20][CH2:19][CH2:18][CH:5]1[CH2:4][C:13]2[C:8](=[C:9]([Cl:17])[C:10]([Cl:16])=[C:11]([O:14][CH3:15])[CH:12]=2)[C:6]1=[O:7]Participants
3
Procedure
2-(Dimethylaminomethyl)-5-chloro-1-(2,3-dichloro-4-methoxyphenyl)-1-pentanone (6.1 g, 0.019 mole) was added in portions to well-stirred concentrated sulfuric acid (25 ml). The temperature rose to 39° C. after which the mixture was stirred at ambient temperature for an additional two hours. The mixture was poured into crushed ice and the resulting precipitate removed by filtration, washed with water, dried and then recrystallized from a mixture of tetrahydrofuran and ether to give 2-(3-chloropropyl)-6,7-dichloro-2,3-dihydro-5-methoxy-1H-inden-1-one, 5 g, m.p. 130°-132° C.
Workup
- customrose to 39° C.
- additionThe mixture was poured
- custominto crushed ice
- customthe resulting precipitate removed by filtration