Ethyl 2-bromoisobutyrate synthesis
- Product Name:Ethyl 2-bromoisobutyrate
- CAS Number:600-00-0
- Molecular formula:C6H11BrO2
- Molecular Weight:195.05
Yield:600-00-0 92.53%
Reaction Conditions:
Stage #1: 2-bromo-2-methylpropionic acidwith zinc for 0.5 h;
Stage #2: with hydrogen bromide for 0.5 h;
Stage #3: ethanol at 95;
Steps:
1; 2; 3 Example 3
Transfer the filtrate to a 500 ml three-necked flask with a thermometer and a stirring paddle.A three-necked flask was fixed to the bottom of the distillation column.Add zinc powder to the three-necked flask: 0.9g, stir for 30 minutes, the color of the material in the three-necked bottle will gradually fade.40% hydrobromic acid was added to the three-necked flask: 1.2 g, stirred for 30 minutes, and then ethanol was added to 33.1 g.(content: 99.0%, 0.7124 mol).The outer wall of the three-necked flask was heated in a water bath, and the water temperature of the water bath was set to 95 °C. Open stirring, warm up the total reflux reaction, reverseThe turbid light component with higher water content is intermittently produced during the process. After 5 to 10 hours of reflux dehydration reaction, sample detectionThe content of the material in the reaction flask is stopped when the content of α-bromoisobutyric acid is less than 3.5%.The outer wall of the reaction bottle is cooled with 20-30 ° C cooling water. When the internal temperature is less than 35 ° C, stirring is stopped and the reaction bottle is placed.The material was transferred to a separatory funnel and the reaction was washed three times with 200 ml of deionized water. After washing, it will be in the separatory funnelThe material was transferred to a 500 ml three-necked flask with a thermometer and a stirring paddle. Three-necked flask was fixed to the recovery unit, three-necked flaskThe outer wall is heated in a water bath, the water temperature of the water bath is set to 80 ° C, and the internal temperature of the reaction bottle is controlled to be ≤ 60 ° C, and the vacuum degree is ≥ 0.06 MPa.The n-hexane was recovered under reduced pressure. After the recovery, 73.4 g of a colorless transparent ethyl α-bromoisobutyrate was obtained (content: 96.8%, yield:92.53%).
References:
CN108997107,2018,A Location in patent:Paragraph 0043; 0047-0049; 0050; 0054-0057; 0061-0063
64-17-5
892 suppliers
$10.00/50g
20769-85-1
276 suppliers
$13.00/5g
600-00-0
258 suppliers
$13.00/5g
97-62-1
284 suppliers
$16.60/100G
600-00-0
258 suppliers
$13.00/5g
79-31-2
460 suppliers
$18.00/25mL
600-00-0
258 suppliers
$13.00/5g