Azobisisobutyronitrile → HCID 86666345, compound

HRID 2273366Notes

Reaction equation

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

Participants

Conditions

Temperature: 60 °C

Procedure

1.31 g (2.88 mmol, 1 eq.) (ethyl 2-[(bis{2,4,6-trimethylbenzoyl}-phosphoryl]-methyl)acrylate (example 2) and 2.98 mL (2.7 g, 25.9 mmol, 9 eq.) styrene are dissolved in 1 ml toluene. 80 mg (2 wt %) AIBN are added to this solution and the solution is stirred at 60° C. for 60 hours. 5 mL Toluene are added to the yellow gel which is formed in order to dissolve the polymer. Subseqeuntly, the polymer is precipitated by the addition of petroleum ether. This procedure is repeated two times and the polymer is filtrated off and washed with petroleum ether. The polymer is dried by vacuum to give 2.3 g of the (ethyl 2-([bis{2,4,6-trimethylbenzoyl}-phosphoryl]-methyl)acrylate/styrene copolymer. Conversion: 55.6%.

Workup

customis formed in order
dissolutionto dissolve the polymer
customSubseqeuntly, the polymer is precipitated by the addition of petroleum ether
filtrationthe polymer is filtrated off
washwashed with petroleum ether
customThe polymer is dried by vacuum

Sources & evidence

ORD record: ord-59beff9630b04341b7ca596b70c0728b
Source dataset: uspto-grants-2015_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09120900B2

Reaction notes

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