BIS(4-CHLOROBUTYL) ETHER synthesis
- Product Name:BIS(4-CHLOROBUTYL) ETHER
- CAS Number:6334-96-9
- Molecular formula:C8H16Cl2O
- Molecular Weight:199.12
110-56-5
306 suppliers
$15.00/25mL
6334-96-9
122 suppliers
$24.69/5g
Yield:6334-96-9 68.08%
Reaction Conditions:
with trichlorophosphate in tetrahydrofuran at 20 - 90; for 0.5 h;
Steps:
1
Step 1. In a 1L three-necked flask, add 180.3g of dried tetrahydrofuran, start stirring, add 126.5g of phosphorus oxychloride dropwise under ice bath; over 20;Step 2. Add 400g of 1,4-dichlorobutane into another 2L three-necked bottle, the internal temperature rises to 70°C, and the mixed solution prepared in steps 1 and 2 is added dropwise, and the internal temperature is controlled at 70-90°C; After the mixed solution was added, the temperature was lowered to 70 °C, 300 g of water was added, and the reflux was continued for 30 minutes;Step 3, remove unreacted tetrahydrofuran and a small amount of by-product 1,4-dichlorobutane formed by azeotropic distillation at atmospheric pressure, the boiling point is 161-163 ° C, steam to a steam temperature of 99-100 ° C to stop; cool to room temperature, replenish Add 160 g of water, separate the oil layer, add 100 g of methyl ether to the water layer for extraction, combine the organic phases, wash with 5% sodium bicarbonate and saturated brine successively; the organic phase is dried over anhydrous sodium sulfate;Step 4: Rotary distillation of methyl tert-butyl ether at atmospheric pressure; vacuum distillation of the residue; the finished product: 86g, yield: 68.08%, b.p.84-86°C/0.5mm.
References:
CN113999091,2022,A Location in patent:Paragraph 0030-0039
109-99-9
1111 suppliers
$9.00/5ml
6334-96-9
122 suppliers
$24.69/5g
109-99-9
1111 suppliers
$9.00/5ml
6334-96-9
122 suppliers
$24.69/5g
110-56-5
306 suppliers
$15.00/25mL
110-63-4
710 suppliers
$24.80/250g
1190-22-3
86 suppliers
$39.00/1g
928-51-8
340 suppliers
$6.00/5g
6334-96-9
122 suppliers
$24.69/5g
110-56-5
306 suppliers
$15.00/25mL
