Application of 102169-44-8, A common heterocyclic compound, 102169-44-8, name is 4-Bromo-5-methylbenzene-1,2-diamine, molecular formula is C7H9BrN2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
4-bromo-5-methylbenzene-1,2-diamine (0.5 g, 2.3 mmol) and cyclopropanecarboxaldehyde (207 mg, 18 mmol) was dissolved in 7.5 ml of ethanol and cobalthydroxide (22 mg, 0.24 mmol) blended. The reaction mixture was stirred overnight, opened the lid, filtered and concentrated under reduced pressure to dryness. The residue was By chromatography were purified (2chiLabomatic HD-3000 spring via HPLC, Labomatic AS-3000> Knauer DAD 2600 5 Labomatic Labcol Vario 4000 Plus Chromatorex C18 10 micron 125 mm chi 30 mm +250 mm chi 50.8 mm; eluent A: water volume +0.2 /. Ammonia (32%), Eluent B: methanol, gradient: 0-12 min 70-100% B; flow rate: 100 ml / min). 184 mg (31% of the theoretical value) of this compound to produce the subject.
The synthetic route of 102169-44-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; ROEHN, ULRIKE; ELLERMANN, MANUEL; STRASSBURGER, JULIA; WENDT, ASTRID; ROEHRIG, SUSANNE; WEBSTER, ROBERTALAN; SCHMIDT, MARTINAVICTORIA; TERSTEEGEN, ADRIAN; BEYER, KRISTIN; SCHAEFER, MARTINA; BUCHMUELLER, ANJA; GERDES, CHRISTOPH; SPERZEL, MICHAEL; SANDMANN, STEFFEN; HEITMEIER, STEFAN; HILLISCH, ALEXANDER; ACKERSTAFF, JENS; TERJUNG, CARSTEN; (148 pag.)TW2016/5809; (2016); A;,
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