Phosphorus trichloride → n-Butyl tert-butyl chlorophosphine

HRID 2360

반응식

HRID 2360 반응식
[P:1]([Cl:4])(Cl)Cl.[C:5]([Mg]Cl)([CH3:8])([CH3:7])[CH3:6].[CH2:11]([Mg]Cl)[CH2:12][CH2:13][CH3:14]>C(OCC)C>[CH2:11]([P:1]([C:5]([CH3:8])([CH3:7])[CH3:6])[Cl:4])[CH2:12][CH2:13][CH3:14]

참가 물질

5

반응물 3

HCID 24387Phosphorus trichlorideHCID 178418265HCID 178418265, 화합물HCID 178418310HCID 178418310, 화합물

생성물 1

HCID 12507378n-Butyl tert-butyl chlorophosphine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
-25 °C

실험 절차

To a solution of phosphorus trichloride (55 g) in dry diethyl ether (200 cm3) stirred and maintained at between -25° C. and -30° C. in an atmosphere of dry nitrogen a 2 molar solution of tert-butyl magnesium chloride in diethyl ether (200 cm3, solution supplied by Aldrich Chemical Co.) was added during 45 min. After a further 30 min., a 2 molar solution of n-butyl magnesium chloride (200 cm3, solution supplied by Aldrich Chemical Co.) was added in the same way. The suspension was stirred at -25° C. for a further 45 min., then allowed to reach ambient temperature, and finally boiled under reflux for 30 min., cooled, filtered to remove magnesium chloride, and distilled, yielding n-butyl tert-butyl chlorophosphine (30.8 g), b.p. 76°-78° C. under a pressure of 15 mm of mercury.

후처리

  1. additionwas added during 45 min
  2. customto reach ambient temperature
  3. temperatureunder reflux for 30 min.
  4. temperaturecooled
  5. filtrationfiltered
  6. customto remove magnesium chloride
  7. distillationdistilled

출처 및 근거

ORD 기록
ord-e7d8772123ce4e13a0605b2c4b96576a
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728853

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