Azobisisobutyronitrile → HCID 86666344, compound

HRID 2273365Notes

Reaction equation

[CH:1]([C:3]1[CH:32]=[CH:31][C:6]([CH2:7][P:8]([C:20](=[O:30])[C:21]2[C:26]([CH3:27])=[CH:25][C:24]([CH3:28])=[CH:23][C:22]=2[CH3:29])[C:9](=[O:19])[C:10]2[C:15]([CH3:16])=[CH:14][C:13]([CH3:17])=[CH:12][C:11]=2[CH3:18])=[CH:5][CH:4]=1)=[CH2:2].[CH2:33]=[CH:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1.CC(N=NC(C#N)(C)C)(C#N)C>C1(C)C=CC=CC=1>[CH:1]([C:3]1[CH:4]=[CH:5][C:6]([CH2:7][P:8]([C:9](=[O:19])[C:10]2[C:15]([CH3:16])=[CH:14][C:13]([CH3:17])=[CH:12][C:11]=2[CH3:18])[C:20](=[O:30])[C:21]2[C:22]([CH3:29])=[CH:23][C:24]([CH3:28])=[CH:25][C:26]=2[CH3:27])=[CH:31][CH:32]=1)=[CH2:2].[CH2:33]=[CH:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1

Participants

Conditions

Temperature: 60 °C

Procedure

0.78 g (1.71 mmol, 1 eq.) of freshly prepared (4-vinylbenzyl)-bis(2,4,6-trimethylbenzoyl)-phosphine (example 1) and 1.8 mL (1.6 g, 15.4 mmol, 9 eq.) styrene are dissolved in 0.6 mL toluene. 47.6 mg (2% w/w) AIBN are added and the solution is stirred at 60° C. for 50 hours. 5 ml Toluene are subsequently added to the yellow gel which is formed in order to dissolve the polymer. The polymer is then precipitated by the addition of petroleum ether. This procedure is repeated twice before the polymer is filtrated off and washed with petroleum ether. The polymer is dried under vacuum providing 2.121 g of the (4-vinylbenzyl)-bis(2,4,6-trimethylbenzoyl)-phosphine/styrene co-polymer. Conversion: 87.4%.

Workup

customis formed in order
dissolutionto dissolve the polymer
customThe polymer is then precipitated by the addition of petroleum ether
filtrationis filtrated off
washwashed with petroleum ether
customThe polymer is dried under vacuum

Sources & evidence

ORD record: ord-7dbbb212ce5f4347935cbbced3fa79f3
Source dataset: uspto-grants-2015_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09120900B2

Reaction notes

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