2-IODO-6-METHYLBENZOIC ACID synthesis
- Product Name:2-IODO-6-METHYLBENZOIC ACID
- CAS Number:54811-50-6
- Molecular formula:C8H7IO2
- Molecular Weight:262.04
4389-50-8
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54811-50-6
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Yield: 79%
Reaction Conditions:
Stage #1:2-amino-6-methylbenzoic acid with hydrogenchloride;sodium nitrite in water at 0 - 5;
Stage #2: with potassium iodide in water at 20; for 16 h;
Steps:
1; 12; A
A solution of 2-amino-6-methylbenzoic acid (1601) (106.5 g, 705 mmol) in H2O (200 mL) was cooled to 0 - 5 0C, con. HCl (250 mL) was added slowly. The solution was stirred for 15 min at 0-5 0C. A solution of sodium nitrite (58.4 g, 6.85 mol) in H2O (120 mL) was added dropwise at 0-5 0C, and the resulting mixture was stirred for 30 min. Then above solution was added to a solution of KI (351 g, 2.11 mol) in H2O (200 mL), and the resulting mixture was stirred at RT for 16 h. The solution was poured into ice water (2000 mL) and extracted with ethyl acetate (3 x 1000 mL). The combined organic layer was washed with aqueous NaOH (15%, 3 x 200 mL). The aqueous layer was acidified to PH = 1, and extracted with ethyl acetate (3 x 1000 mL). The combined organic layer was dried over
References:
Location in patent:Page/Page column 78-79
118-90-1
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54811-50-6
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$58.00/250mg
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54811-50-6
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