4-(4-BROMOPHENOXY)BENZOIC ACID 97 synthesis

12synthesis methods

Product Name:4-(4-BROMOPHENOXY)BENZOIC ACID 97
CAS Number:21120-68-3
Molecular formula:C13H9BrO3
Molecular Weight:293.11

21120-75-2
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$97.00/100mg

21120-68-3
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$54.00/1g

Yield:21120-68-3 99.1%

Reaction Conditions:

with lithium hydroxyde monohydrate;water monomer in tetrahydrofuran;methanol at 0 - 20; for 2 h;

Steps:

1.3 Step 3: 4-(4-bromophenoxy)benzoic acid (E).

To a solution of compound D (3.8 g, 12.4 mmol) in MeOH (20 mL), THF (10 mL) and water (10 mL) was added LiOH·H₂O (2.6 g, 61.9 mmol) at 0 °C and the mixture was stirred at room temperature for 2 hours. The mixture was concentrated to 1/5 volume, diluted with water and washed with MTBE twice. The aqueous layer was acidified with 1 N aq. HCl to pH ~3 and extracted with DCM twice. The combined organic layers were washed with brine, dried over anhydrous Na₂SO₄, filtered, and concentrated to dryness under reduced pressure to give compound E (3.6 g, yield 99.1%) as a white solid, which was used directly in next step without further purification. LC/MS (ESI) (m/z): 291/293 (M-H)-.

References:

WO2022/66774,2022,A1 Location in patent:Page/Page column 239; 316-317

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