Water → 3-(4-Bromophenyl)propane-1,2-diol
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH:9]2[CH2:11][O:10]2)=[CH:4][CH:3]=1.C(O)(=O)C(O)=[O:14].O>O1CCOCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH:9]([OH:14])[CH2:11][OH:10])=[CH:6][CH:7]=1参加物
5
実験手順
A mixture of 90 parts of 2-(4-bromophenylmethyl)oxirane, 8 parts of ethanedioic acid, 100 parts of water and 300 parts of 1,4-dioxane is stirred and refluxed overnight. The reaction mixture is evaporated. The residue is dissolved in trichloromethane. The solution is washed with 110 parts of a sodium hydroxide solution 10%, dried, filtered and evaporated. The residue is distilled (bp. 165° C. at 0.6 mm. pressure). The distillate is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 25 parts of 3-(4-bromophenyl)-1,2-propanediol; mp. 60.6° C.
後処理
- temperaturerefluxed overnight
- customThe reaction mixture is evaporated
- dissolutionThe residue is dissolved in trichloromethane
- washThe solution is washed with 110 parts of a sodium hydroxide solution 10%
- customdried
- filtrationfiltered
- customevaporated
- distillationThe residue is distilled (bp. 165° C. at 0.6 mm. pressure)
- customThe distillate is crystallized from 2,2'-oxybispropane
- filtrationThe product is filtered off
- customdried
出典と根拠
- ORDレコード
- ord-9fcf281e08ed45539568104f5be29b82
- 出典データセット
- uspto-grants-1978_10
- 特許番号
- US04120869
反応ノート
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