6,7-DICHLORO-1,2,3,4-TETRAHYDROISOQUINOLINE synthesis
- Product Name:6,7-DICHLORO-1,2,3,4-TETRAHYDROISOQUINOLINE
- CAS Number:75416-52-3
- Molecular formula:C9H9Cl2N
- Molecular Weight:202.08
73075-49-7
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Yield:75416-52-3 47%
Reaction Conditions:
with sodium hydrogencarbonate in dichloromethane;water;
Steps:
6,7-dichloro-1,2,3,4-tetrahydroisoquinoline HCl salt (550 mg, 2.31 mmol) was dissolved in water (5 mL) and DCM (20 mL). Aqueous saturated NaHCO3 (10 mL) was added and the organic phase was separated. The aqueous phase was extracted twice with DCM (20 mL), the organic phases were combined, dried (Na2SO4), and filtered to give 6,7-dichloro-1,2,3,4-tetrahydro-isoquinoline (470 mg, quant.). Purification Method B The crude free base residue obtained was purified by silica-gel column chromatography (120 g, 4% MeOH in DCM) providing 6,7-dichloro-1,2,3,4-tetrahydroisoquinoline (3.0 g, 47%). hu 1H NMR (400 MHz, CDCl3) δ ppm: 7.20 (s, 1H), 7.12 (s, 1H), 3.96 (s, 2H), 3.12 (dd, J=6.0, 6.0 Hz, 2H) and 2.75 (dd, J=5.9, 5.9 Hz, 2H). LC/MS (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)), m/z: M+1 obs=202.3; tR=0.82 min.
References:
US2009/124655,2009,A1 Location in patent:Page/Page column 29
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