تفاعل #572406
ord-484804a6c0c94b3ea6e8b39d334ae63c
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىAfter the exothermal reaction which
- 2أخرىwas terminated
- 3أخرىThe yields (31 -P-NMR)
- 4workup.DISTILLATIONThe crude product was distilled
الإجراء التجريبي
19.8 g (0.1 mol) dicyclohexylphosphane was added dropwise at room temperature to 26.1 g (0.11 mol) hexachloroethane. After the exothermal reaction which took place with evolution of HCl was terminated, the reaction mixture was stirred for 3 hours at 100° C. The yields (31 -P-NMR) were as follows: δ P=125.2 ((C6H11)2PCl, 94 wgt %); δ P=194.4 (C6H11PCl2, 2 wgt %); δ P=76.7 ((C6H11)2P(O)Cl, 4 wgt %). The crude product was distilled and 13.7 g (59 wgt %) dicyclohexylchlorophosphane (bp.: 136°-138° C./4 millibars) was obtained.