Thionyl Chloride → 3,5-Dichlorobenzyl chloride
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:10])[CH:9]=1)[CH2:5]O.S(Cl)([Cl:13])=O>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:10])[CH:9]=1)[CH2:5][Cl:13]参加物
4
実験手順
A mixture of 3,5-dichlorobenzyl alcohol (Aldrich, 25 g) , thionyl chloride (100 ml) and DMF (0.5 ml) was stirred and refluxed for 4 hours. After cooling the mixture was concentrated in vacuo, the residue was taken up in ether, washed with saturated aqueous NaHCO3 and brine, dried (MgSO4) and concentrated in vacuo to give 3,5-dichlorobenzyl chloride as a light yellow solid, which was used without further purification, 28 g, mp. 32°-36° C.
後処理
- temperaturerefluxed for 4 hours
- temperatureAfter cooling the mixture
- concentrationwas concentrated in vacuo
- washwashed with saturated aqueous NaHCO3 and brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-0e68d73215e841639b2447213a833f42
- 出典データセット
- uspto-grants-1997_01
- 特許番号
- US05597827
反応ノート
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