Hexane → HCID 68953581, compound

HRID 659926Notes

Reaction equation

[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][C:12](=[O:14])[CH3:13])[CH:6]=[CH2:7].C(OC1C=CC(C=C)=CC=1)(=O)C.N(C(C)(C)C(OC)=O)=NC(C)(C)C(OC)=O.CCCCCC>O1CCCC1>[C:12]([O:11][C:10]1[CH:9]=[CH:8][C:5]([CH:6]=[CH2:7])=[CH:4][CH:3]=1)(=[O:14])[CH3:13].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][C:12](=[O:14])[CH3:13])[CH:6]=[CH2:7]

Participants

Conditions

Temperature: 65 °C

Procedure

In a reaction vessel, 96.1 g (0.5 mol) of 3-methoxy-4-acetoxystyrene (manufactured by Honshu Chemical Industry Co., Ltd.) and 81.1 g (0.5 mol) of 4-acetoxystyrene (manufactured by Honshu Chemical Industry Co., Ltd.) are dissolved in 400 ml of tetrahydrofuran, and nitrogen gas is streamed to the reaction solution while stirring. To the solution is added 23.0 g (0.1 mol) of polymerization initiator V-601 (manufactured by Wako Pure Chemical Industries), and the reaction solution is heated at 65° C. After stirring for 10 hours, the reaction solution is allowed to cool to room temperature and then dropped into 5 liters of hexane to precipitate a polymer. A filtered solid is dissolved in 600 ml of acetone, dropped again into 5 liters of hexane and a filtered solid is dried under reduced pressure to obtain 150.6 g of a (3-methoxy-4-acetoxystyrene)-(4-acetoxystyrene) copolymer.

Workup

additionTo the solution is added
stirringAfter stirring for 10 hours
temperatureto cool to room temperature
customto precipitate a polymer
dissolutionA filtered solid is dissolved in 600 ml of acetone
additiondropped again into 5 liters of hexane
customa filtered solid is dried under reduced pressure

Sources & evidence

ORD record: ord-19e399ef823942daa3d6e69823112bf0
Source dataset: uspto-grants-2011_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08084183B2

Reaction notes

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