1-Bromo-3-methylnaphthalene synthesis
- Product Name:1-Bromo-3-methylnaphthalene
- CAS Number:54357-18-5
- Molecular formula:C11H9Br
- Molecular Weight:221.09
37113-08-9
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Yield:54357-18-5 91%
Reaction Conditions:
Stage #1: amino-1 bromo-4 methyl-2 naphtalenewith hydrogenchloride;glacial acetic acid;NaNO2 in lithium hydroxide monohydrate at 0; for 1 h;
Stage #2: with hypophosphorous acid in lithium hydroxide monohydrate at 20; for 18 h;
Steps:
70.5 Step 5:
C085-4 (100 mg, 0.43 mmol) was dispersed in acetic acid (2 mL) and hydrochloric acid (0.2 mL), cooled to about 0 degrees, and an aqueous solution of sodium nitrite (32 mg, 0.47 mmol) was added dropwise. After the reaction for 1 h, the diazonium salt solution was poured into an aqueous solution of hypophosphorous acid (5 mL, 50%), and the reaction was carried out at room temperature for 18 h. TLC detected that the reaction was complete.The reaction solution was poured into ice water, extracted with PE/EA, and the organic phases were combined.Washed with saturated brine, dried over anhydrous sodium sulfate, concentrated, and the crude product was purified by silica gel column chromatography to obtain colorless oil C085-5 (85 mg, yield 91%).
References:
WO2022/17531,2022,A1 Location in patent:Page/Page column 87-88
13615-35-5
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54357-18-5
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82670-06-2
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54357-18-5
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13615-38-8
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54357-18-5
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54357-18-5
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