Сообщение
slavert » Вт окт 17, 2006 2:49 pm
Bibliographic Information
Aminosulfenyl halides. (Farbenfabriken Bayer A.-G.). (1958), GB 790021 19580129 Patent language unavailable. CAN 52:77528 AN 1958:77528 CAPLUS
Patent Family Information
Patent No. Kind Date Application No. Date
GB 790021 19580129 GB 1955-31497 19551103
Abstract
Aminosulfenyl halides, R1R2NSX, are prepd. by treating an amino disulfide with a chlorinating or brominating agent. Thus, 100 g. dimorpholino disulfide is suspended in 800 cc. dry CCl4 and dry Cl fed in at 0-5° until a small excess is present. After 1-2 min. a test is made with KI starch paper. If the test is pos. the excess Cl is removed in vacuo at 0-5° or by an inert gas. The resultant light orange soln. is mixed with C and after filtration the solvent distd. in vacuo at 30-40° and finally at 50°. The yield is 92% red-brown compd. Morpholinosulfenyl chloride is obtained on vacuum distn. as an orange colored fluid, b0.5 64-6°. Piperidinosulfenyl chloride, b0.3 44-5°, piperidinosulfenyl bromide, b0.4 65-8°, thiamorpholinosulfenyl bromide, b0.45 103-5°, diethylaminosulfenyl chloride, b13 62-4°, dibutylaminosulfenyl chloride, b0.45 75-6°, diisobutylaminosulfenyl chloride, b0.45 61-4°, tert-octyl-n-propylaminosulfenyl chloride, b0.1 86-8°, b,b'-dichlorodiethylaminosulfenyl chloride, b0.1 88-90°, cyclohexylethylaminosulfenyl chloride, b0.4 90-2°, dicyclohexylaminosulfenyl chloride, dibenzylaminosulfenyl chloride, and tetrahydroisoquinolinosulfenyl chloride are obtained in a similar manner.