7-methoxy-2,3-dihydro-1H-inden-1-amine synthesis
- Product Name:7-methoxy-2,3-dihydro-1H-inden-1-amine
- CAS Number:1032279-33-6
- Molecular formula:C10H13NO
- Molecular Weight:163.22
908108-58-7
1032279-33-6
Step A: Synthesis of racemic-7-methoxy-indan-1-ylamine A mixture of 7-methoxy-indan-1-one oxime (CAS 908108-58-7, containing (E)-oxime, CAS 179899-16-2) (22.3 g, 126 mmol) was reacted with nickel ryenne (11.26 g) in a mixture of solvents of tetrahydrofuran (570 mL) and methanol (570 mL) at 100 bar of hydrogen pressure at 60 °C for Hydrogenation reaction was carried out for 22 hours. Upon completion of the reaction, the catalyst was removed by filtration and washed with methanol and tetrahydrofuran. Subsequently, all volatiles were removed by vacuum distillation to afford 7-methoxy-1-indenamine as a brown oil (19.95 g, 97% yield, HPLC retention time 0.4 min). Mass spectrometry (ISP) analysis showed m/e = 164.2 [(M+H)+].
908108-58-7
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1032279-33-6
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Yield:1032279-33-6 97%
Reaction Conditions:
with hydrogen;Raney-Nickel in tetrahydrofuran;methanol at 60; under 75007.5 Torr; for 22 h;
Steps:
10.A rac-N2-(7-Methoxy-indan-1-yl)-4H-benzo[d][1,3]oxazine-2,6-diamine
Step A: rac-7-Methoxy-indan-1-ylamine A mixture of 7-methoxy-indan-1-one oxime (CAS 908108-58-7, (E)-oxime 179899-16-2) (22.3 g, 126 mmol)) and Raney-Nickel (11.26 g) in tetrahydrofuran (570 mL) and methanol (570 mL) was hydrogenated at 100 bar hydrogen-pressure at 60° C. for 22 h. Filtered the catalyst off, washed with methanol and tetrahydrofuran, all volatiles were removed in vacuum to give the title compound as a brown oil (19.95 g, 97%, HPLC 0.4 min), MS (ISP) m/e=164.2 [(M+H)+].
References:
US2010/63037,2010,A1 Location in patent:Page/Page column 23
1187160-18-4
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1032279-33-6
24 suppliers
$223.00/100mg
928169-32-8
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1032279-33-6
24 suppliers
$223.00/100mg