4-broMo-2-Methylfuran synthesis
- Product Name:4-broMo-2-Methylfuran
- CAS Number:24666-43-1
- Molecular formula:C5H5BrO
- Molecular Weight:161
21921-76-6
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Yield:-
Reaction Conditions:
Stage #1: 4-bromo-2-furancarbaldehydewith hydrazine in diethyl ether at 20; for 0.0833333 h;
Stage #2: with calcium chloride in diethyl ether at 20; for 1 h;
Stage #3: with sodium ethanolate in ethanol at 90; for 2 h;
Steps:
5.b
4-Bromo-2-furaldehyde (220 mg, 1.26 mmol) and hydrazine (161 mg, 5.03 mmol) were stirred in 3 mL of anhydrous ether at room temperature for 5 minutes. Then calcium chloride (168 mg, 1.51 mmol) was added, and the mixture was stirred for lh. The mixture was filtered, and the filtrate was evaporated. The residue was dissolved in 2 mL of anhydrous ethanol, and sodium ethoxide (685 mg, 10.1 mmol) was added. The reaction was heated at 90 °C for 2 h. The mixture was diluted with a large amount of water, and extracted with pentane. The organic layer was washed with water and brine, and dried through MgS04. Because the product was very volatile, the product-containing solution was used for step (c) without evaporation of further purification ; m/e 160,162 (M+).
References:
WO2003/87102,2003,A1 Location in patent:Page/Page column 17
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24666-43-1
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