Toluene → Tributylphosphine

HRID 2285835Notes

Reaction equation

HRID 2285835 reaction equation
[PH3:1].[C:2]1([CH3:8])[CH:7]=[CH:6]C=CC=1>>[CH2:6]([P:1]([CH2:6][CH2:7][CH2:2][CH3:8])[CH2:8][CH2:2][CH2:7][CH3:6])[CH2:7][CH2:2][CH3:8]

Participants

3

Procedure

0.52 kg PH3 and 2.6 kg butene-(1) were reacted as described in Example 7 to give an about 50% solution of tri-n-butyl-phosphine in toluene. Introduced thereinto under slight overpressure were 16.2 kg butene-(1) and 2.82 kg PH3. The whole was heated to about 70° C. and initiator solution was metered thereinto. The exothermal reaction made the temperature increase to 106° C. and the pressure to 23 bars. Altogether 3 l initiator solution was added within 3 hours. The pressure was then found to have dropped to 5 bars (at 120° C.). The whole was allowed to cool, a specimen was taken and analyzed gas-chromatographically. It was an about 67% tributylphosphine solution in toluene, corresponding to a conversion rate of more than 95%, based on butene and PH3.

Sources & evidence

ORD record
ord-e411a985e97d4c1e88173c24cb2d603a
Source dataset
uspto-grants-1982_04
Patent number
US04324919

Reaction notes

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