Diethylamine → Chlorobis(diethylamino)phosphine

HRID 564283

반응식

HRID 564283 반응식
[P:1]([Cl:4])(Cl)Cl.[CH2:5]([NH:7][CH2:8][CH3:9])[CH3:6]>C(OCC)C>[Cl:4][P:1]([N:7]([CH2:8][CH3:9])[CH2:5][CH3:6])[N:7]([CH2:8][CH3:9])[CH2:5][CH3:6]

참가 물질

4

반응물 2

HCID 8021DiethylamineHCID 24387Phosphorus trichloride

생성물 1

HCID 2733351Chlorobis(diethylamino)phosphine수율 78%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a solution of phosphorous trichloride (26 ml; 0.298 mol) in dry diethylether (500 ml) at −78° C., acetone/CO2 bath, under dry nitrogen gas atmosphere was added diethylamine (123.4 ml; 1.19 mol) dropwise via a pressure equalised dropping funnel over 2 hrs. A thick suspension formed, reaction allowed to warm to ambient temperature and stirred for an additional 2 hrs. After this time the suspension was filtered under dry nitrogen gas via an oven dried filter stick, washing with dry diethylether (3×100 ml). Filtrate was evaporated under high vacuum on the Schlenk line, using a cold-finger trap to condense solvent vapours, to give an oil. The oil was purified by distillation under reduced pressure to give the required product (b.p. 105° C. @ 10 mmHg; 49 g; 70% yield). 1H NMR (300 MHz, CDCl3), δ/ppm; 1.08 (6H, t J=7.0, CH3), 3.08 (4H, ap. br. d J=7.0, CH2); 31P NMR (121 MHz, CDCl3) δ/ppm; 159.9.

후처리

  1. customover 2 hrs
  2. customA thick suspension formed
  3. customreaction
  4. filtrationAfter this time the suspension was filtered under dry nitrogen gas via an oven
  5. customdried
  6. filtrationfilter stick
  7. washwashing with dry diethylether (3×100 ml)
  8. customFiltrate was evaporated under high vacuum on the Schlenk line
  9. customto condense solvent vapours
  10. customto give an oil
  11. distillationThe oil was purified by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-266d3613137d4784a0499e0f4ff1de57
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067642B2

연결된 노트

불러오는 중…