Bischloromethyl ether could be produced through the following synthetic routes.

In a 1-l. three-necked flask immersed in an ice bath and provided with a stirrer, thermometer, and dropping funnel are placed 168 ml. (200 g.) of concentrated (37–38%) hydrochloric acid (2 moles) and 240 g. of paraformaldehyde (effectively 8 moles of formaldehyde). While the temperature is maintained below 10°, 452 ml. (6.9 moles) of chlorosulfonic acid is added dropwise at such a rate that gaseous hydrogen chloride is not lost from the mixture. This requires about 5.5 hours. The mixture is stirred for 4 hours in the melting ice bath and comes to room temperature. It may be allowed to stand overnight. The layers are separated, and the product (upper layer) is washed twice with ice water. Ice is added to the product, and 250 ml. of 40% sodium hydroxide is then added to the mixture slowly with vigorous agitation until the aqueous phase is strongly alkaline. The product is separated and dried rapidly over potassium carbonate and then over potassium hydroxide, keeping the product cold during drying. After separation of the drying agent by filtration, 350–370 g. (76–81%) of product sufficiently pure for many purposes is obtained. On distillation there is obtained 330–350 g. (72–76%) of bischloromethyl ether, boiling at 100–104°. Approximately 95% boils at 101–101.5°, n²⁵D 1.4420.

Notice: It has been reported that exposure to bischloromethyl ether in low concentrations has caused severe irritation of the eyes and respiratory tract, and perhaps pulmonary edema.

Proper safeguards should be taken to prevent exposure to this material both during and after its preparation. It is recommended that all operations involving this compound be carried out in a good hood.