7-METHOXY-1,3-BENZODIOXOLE-5-ETHANAMINE synthesis
- Product Name:7-METHOXY-1,3-BENZODIOXOLE-5-ETHANAMINE
- CAS Number:23693-38-1
- Molecular formula:C10H13NO3
- Molecular Weight:195.22
36200-29-0
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23693-38-1
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Yield:23693-38-1 96.5%
Reaction Conditions:
Stage #1: 2-(7-methoxybenzo[d][1,3]dioxol-5-yl)acetonitrilewith hydrogenchloride;hydrogen;platinum(IV) oxide in ethanol;water at 20; under 2068.65 Torr; for 18 h;
Stage #2: with sodium hydroxide in ethanol;water; pH=13 - 14;
Steps:
To a mixture of ethanol (EtOH) (20 mL) , water (8 mL) and IN HCl (2 mL) was added PtO2 (200 mg) and compound A0061-6 (630 mg, 3.56 mmol) and the reaction mixture was hydrogenated overnight (about 18 hours) under 40 psi of H2 at room temperature. Thin- layer chromatography showed the reaction was complete. The solution was concentrated under reduced pressure. To the residue was added water and IM NaOH until the solution reached pH=13~14. The resulting mixture was extracted with CH2Cl2. The organic layer was dried over Na2SO4 and concentrated to give compound A0061-7. (670mg, yield: 96.5%, 1H NMR confirmed) as brown oil.
References:
WO2010/51374,2010,A1 Location in patent:Page/Page column 126
5780-07-4
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121-33-5
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5438-36-8
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3934-87-0
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