4-AMINO-3,5-DIIODOBENZOIC ACID METHYL ESTER synthesis
- Product Name:4-AMINO-3,5-DIIODOBENZOIC ACID METHYL ESTER
- CAS Number:131755-87-8
- Molecular formula:C8H7I2NO2
- Molecular Weight:402.96
619-45-4
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Yield:131755-87-8 83%
Reaction Conditions:
with Iodine monochloride in dichloromethane; for 4 h;Inert atmosphere;Reflux;
Steps:
4
(29 ml., 0.554 mol) dissolved into 500 ml, dichloromcthanc under N2. 4-Amino-methylbcnzoate (33,35 g, 0.221 mol) was added into the reaction mixture slowly. The reaction mixture was heated to reflux for 4 hours. The addition of an additional 500 mL dichloromcthane dissolved the precipitate after cooling to room temperature. The reaction mixture was stirred for 1 hour and then washed with 400 mL saturated aqueous solution of Na2S2< followed by water washing the organic layer twice. The organic fractions were combined and concentrated to about I L. After rccryslallization the product then was collected as needle-like yellow crystals (72.5 g, 83 %). 111 MR (400 Ml Iz, CDCI3): S (ppm): 8.28 (s, 211), 5.04 (s, br, 2H), 3.84 (s, 311).
References:
WO2014/11477,2014,A1 Location in patent:Page/Page column 35
150-13-0
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