ASISCHEM A93504 synthesis
- Product Name:ASISCHEM A93504
- CAS Number:482308-06-5
- Molecular formula:C11H16N2O2
- Molecular Weight:208.26
97459-72-8
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482308-06-5
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$60.00/40mg
Yield:482308-06-5 85%
Reaction Conditions:
with iron(0);ammonia hydrochloride in ethanol;lithium hydroxide monohydrate at 85; for 3 h;
Steps:
Synthesis of 3-methoxy-4-morpholinoaniline (02)
To a stirred solution of 4-(2-methoxy-4-nitrophenyl) morpholine (01) (8 g, 33.5 mmol, 1 eq) in Ethanol ThO (2: 1 ) (120 mL), was added NH4CI (8.93 g, 167 mmol, 5 eq), Fe powder (9.32 g, 167 mmol, 5 eq). The reaction mixture was stirred at 85°C for 3h. After completion of reaction by TLC, the reaction mixture was filtered through Celite pad and washed with EtOAc (200 mL). The filtrate was washed with brine (50 mL), dried over sodium sulfate and concentrated under reduced pressure to afford 3-methoxy-4-morpholinoaniline (02) (6 g, yield: 85%) as brown solid. TLC system MeOH:DCM{ 10:90), Rf value:0.2; LCMS (m/z): 209.2 (M+H)+;’HNMR (400 MHz, DMSO-r) d 6.60 (d, J= 8.4 Hz, 1H), 6.23 (d, J= 2.4 Hz, 1H), 6.07 (dd, J= 2.4 Hz, 8.0 Hz, 1H), 4.72 (s, 2H), 3.68 (s, 3H), 3.66 (t, J= 4.8 Hz, 4H), 2.77 (t, J = 4.8 Hz, 4H).
References:
WO2020/190912,2020,A1 Location in patent:Paragraph 00338-00339
2139-44-8
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482308-06-5
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454-16-0
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482308-06-5
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