Styrene → Styrene
Reaction equation
OCN1[C:7](=O)[C:6]2=[CH:9][CH:10]=[CH:11][CH:12]=[C:5]2[C:4]1=O.[C:14](OC(=O)C)(=O)C.[CH2:21]=[CH:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[CH:29]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=1[CH:37]=[CH2:38])=[CH2:30]>ClC(Cl)C>[CH2:21]=[CH:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[CH:29]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=1[CH:37]=[CH2:38])=[CH2:30].[CH3:21][CH2:22][CH2:23][CH2:7][CH2:6][CH2:9][CH2:10][CH2:11][CH2:12][CH:5]([CH3:4])[CH3:14]Participants
Conditions
- Temperature
- 60 °C
Procedure
354 g of N-hydroxymethyl phthalimide, dissolved in 1200 g of dichlorethane, are heated for 5 hours to reflux temperature with 227 g of acetic acid anhydride. After cooling to 60° C, 150 g of a macroporous styrene polymer crosslinked with 8 % of divinyl benzene (obtained by the bead polymerisation of styrene and divinyl benzene in the presence of 60 % by weight of isododecane, based on the sum total of monomers) are swollen in this solution over a period of 30 minutes. The mixture is then heated to reflux temperature, followed by the dropwise addition with stirring over a period of 4 hours of 240 g of concentrated sulphuric acid. After stirring for another 20 hours at the same temperature, the reaction product is separated off and freed from the dichlorethane adhering to it by suspension in aqueous ammonia solution, followed by azeotropic distillation, in the same way as described in Example 1. The polymer is then heated for 10 hours to 180° C with 40 % sodium hydroxide solution in an autoclave. After the sodium hydroxide has been washed out, 540 ml of a weakly basic anion exchanger are obtained with an acid-binding capacaty for N/10 hydrochloric acid of 2.4 Val/1 and a nitrogen content of 10.6 % in the dry material.
Workup
- temperatureare heated for 5 hours
Sources & evidence
- ORD record
- ord-e569b84992bf46eb955aa93a5d27fc9a
- Source dataset
- uspto-grants-1976_11
- Patent number
- US03989650
Reaction notes
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