Ethylene Glycol → HCID 19434044、化合物
反応式
[Br:1][C:2]1[CH:6]=[C:5]([Br:7])[S:4][C:3]=1[CH:8]=[O:9].[CH2:10](O)[CH2:11][OH:12]>C1(C)C=CC=CC=1.CC1C=CC(S(O)(=O)=O)=CC=1>[Br:1][C:2]1[CH:6]=[C:5]([Br:7])[S:4][C:3]=1[CH:8]1[O:12][CH2:11][CH2:10][O:9]1参加物
5
実験手順
A mixture consisting of the product from Step A (11.0 g, 40.7 mmol), TsOH (0.25 g) and ethylene glycol (5.06 g, 81.5 mmol) in toluene (150 mL) was heated at reflux temperature for 1.5 h, water was removed by a Dean-Stark trap. The reaction mixture was cooled and poured into a saturared aqueous solution of sodium bicarbonate (100 mL). The organic layer was separated, dried (MgSO4), and evaporated to dryness. Purification of this crude material by column chromatography (silica, 6% ethyl acetate/hexane) gave 10.33 g of an oil (81%).
後処理
- temperaturewas heated
- temperatureat reflux temperature for 1.5 h
- customwater was removed by a Dean-Stark trap
- temperatureThe reaction mixture was cooled
- additionpoured into a saturared aqueous solution of sodium bicarbonate (100 mL)
- customThe organic layer was separated
- dry with materialdried (MgSO4)
- customevaporated to dryness
- customPurification of this crude material by column chromatography (silica, 6% ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-8d264e1dad26489098f8308b37e4c13c
- 出典データセット
- uspto-grants-1996_07
- 特許番号
- US05538966
反応ノート
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