Iodoethane → HCID 18958205, compound

HRID 1033269Notes

Reaction equation

HRID 1033269 reaction equation
[C:1]1([CH3:22])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[P:7]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH3:21])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:14].[CH2:23]([I:25])[CH3:24]>C1(C)C=CC=CC=1>[I-:25].[CH2:23]([P+:7]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH3:21])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:14])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=1[CH3:22])[CH3:24]

Participants

4

Conditions

Temperature
27 °C

Procedure

Into a 50 milliliter glass reactor equipped with a thermometer connected to a temperature controller, a heating mantle, a condenser and a magnetic stirring bar, are charge 5 gms (0.0164 mole) of tri-o-tolylphosphine and 23 gms of toluene. The slurry is heated to 27° C. then 3.08 gms (0.0197 mole) of ethyl iodide is added. This reaction mass is heated to 70° C. and maintained for 17 hours, then heated to 100° C. and maintained for 9 hours, then cooled to 70° C. and maintained for 15 hours, then cooled to 26° C. This mixture is filtered and washed with 6 gms of toluene. After vacuum drying, 1.6 gms of ethyltri(o-tolyl)phosphonium iodide is obtained which has a melting point of 247° C. to 250° C.

Workup

  1. customInto a 50 milliliter glass reactor equipped with a thermometer
  2. temperatureThis reaction mass is heated to 70° C.
  3. temperaturemaintained for 17 hours
  4. temperatureheated to 100° C.
  5. temperaturemaintained for 9 hours
  6. temperaturecooled to 70° C.
  7. temperaturemaintained for 15 hours
  8. temperaturecooled to 26° C
  9. filtrationThis mixture is filtered
  10. washwashed with 6 gms of toluene
  11. customAfter vacuum drying

Sources & evidence

ORD record
ord-14e4e882391a44b08af598d0efca206e
Source dataset
uspto-grants-1994_05
Patent number
US05310853

Reaction notes

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