Phosphorus trichloride → n-Butyl tert-butyl chlorophosphine

HRID 2360

反応式

HRID 2360 の反応式
[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]

参加物

5

反応物 3

HCID 24387Phosphorus trichlorideHCID 178418265HCID 178418265、化合物HCID 178418310HCID 178418310、化合物

生成物 1

HCID 12507378n-Butyl tert-butyl chlorophosphine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
-25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e7d8772123ce4e13a0605b2c4b96576a
出典データセット
uspto-grants-1998_03
特許番号
US05728853

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