ChemicalBook CAS DataBase List BIS(4-CHLOROBUTYL) ETHER

BIS(4-CHLOROBUTYL) ETHER synthesis

14synthesis methods

Product Name:BIS(4-CHLOROBUTYL) ETHER
CAS Number:6334-96-9
Molecular formula:C8H16Cl2O
Molecular Weight:199.12

110-56-5 Synthesis

110-56-5
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$15.00/25mL

6334-96-9
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$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 Synthesis