Benzenemethanamine, 4-fluoro-3-methoxy- (9CI) synthesis
- Product Name:Benzenemethanamine, 4-fluoro-3-methoxy- (9CI)
- CAS Number:508177-67-1
- Molecular formula:C8H10FNO
- Molecular Weight:155.17
243128-37-2
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$7.00/1g
508177-67-1
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$325.00/5g
Yield:508177-67-1 100%
Reaction Conditions:
with hydrogen;acetic acid;palladium 10% on activated carbon under 3112.81 Torr; for 8 h;
Steps:
98
Preparation 98; 4-Fluoro-3-methoxy-benz lamine; Add 4-fluoro-3-methoxy-benzonitrile (2 g, 0. 01 mol), 10% palladium on carbon (0.400 g) and glacial acetic acid (120 ml) to a pressure vessel. Purge the reaction vessel with nitrogen, purge the reaction vessel with hydrogen, pressurize the reaction mixture with hydrogen (415 Kpa), seal the vessel, and agitate the reaction. After 8 hours stop the agitation, vent the excess hydrogen from the vessel and purge the vessel with nitrogen. Filter the reaction mixture to remove the 5% palladium on carbon and return the filtrate for product isolation. Concentrate the crude solution, re-dissolve in CH2C12 (80mL) and washe with 5N NaOH (35mL). Separate the organic and aqueous phases and extract the aqueous with additional CHUCK (20mL). Combine the organic solutions, dry, filter and concentrate to give the crude material 2. 08g (100%). The title compound as the major product (Rf = 0.12, 10% MeOH/CH2C12) is used without further purification. MS (ES+) 156.1 (M+1) +. lH NMR (400MHz, CDC13) : 8 7. 01 (dd, 1H, J= 8.2, 11.4), 6.95 (dd, 1H, J = 2. 1,8. 4), 6.80 (m, 1H), 3.89 (s, 3H), 3.82 (s, 2H), 1.54 (br s, 2H).
References:
WO2005/66126,2005,A1 Location in patent:Page/Page column 81-82
128495-46-5
222 suppliers
$8.00/1g
508177-67-1
54 suppliers
$325.00/5g