1-Butene → Tributylphosphine

HRID 845324Notes

Reaction equation

HRID 845324 reaction equation
[CH3:1][CH2:2][CH:3]=[CH2:4].[PH3:5]>C1(C)C=CC=CC=1>[CH2:4]([P:5]([CH2:1][CH2:2][CH2:3][CH3:4])[CH2:4][CH2:3][CH2:2][CH3:1])[CH2:3][CH2:2][CH3:1]

Participants

4

Reactant 2

HCID 78441-ButeneHCID 24404Phosphine

Product 1

HCID 13831Tributylphosphine

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Conditions

Temperature
80 °C

Procedure

A 90 liter-autoclave was charged with 9.6 kg (170 mol) butene-1 and 1.75 kg (51 mol) PH3 in the sequential order indicated. Next, the autoclave was heated to 80° C. and the addition of the toluene/ABIN-solution was started. 12 l toluene in which 170 g ABIN (2 mol %, based on PH3) was dissolved was pumped over a period of 2.5 hours into the reactor so that the temperature of the reaction mixture did not exceed 100° C. After a reaction period of 71/2 hours, the whole was allowed to cool and the crude product (18.3 kg) was given into a barrel scavenged with nitrogen.

Workup

  1. customdid not exceed 100° C
  2. temperatureto cool

Sources & evidence

ORD record
ord-33c4002864834be5903a05008949e10f
Source dataset
uspto-grants-1988_07
Patent number
US04757156

Reaction notes

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