Methanol → HCID 28879848、化合物
反応式
[C:1]([C:3]1[CH:14]=[CH:13][C:6]([O:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[CH:5][CH:4]=1)#[N:2].S(Cl)(Cl)=O.[CH3:19]O>>[C:1]([C:3]1[CH:14]=[CH:13][C:6]([O:7][CH2:8][CH2:9][C:10]([O:12][CH3:19])=[O:11])=[CH:5][CH:4]=1)#[N:2]参加物
4
実験手順
A solution of 3.80 g (19.9 mmol) of 3-(4-cyanophenoxy)propanoic acid in 10 ml of methanol is cooled by an ice bath. 3 ml (40 mmol) of thionyl chloride are added drop by drop and then the reaction medium is agitated with solvent reflux for 2 hours. The reaction mixture is then concentrated under reduced pressure and the evaporation residue is purified by silica column chromatography eluting with the help of a dichloromethane/methanol mixture (99/1; v/v). The expected product is obtained in the form of a white solid with a yield of 79%.
後処理
- temperaturereflux for 2 hours
- concentrationThe reaction mixture is then concentrated under reduced pressure
- customthe evaporation residue is purified by silica column chromatography
- washeluting with the help of a dichloromethane/methanol mixture (99/1; v/v)
出典と根拠
- ORDレコード
- ord-e07b5f85bb9342fbb34a13bb02cfdf27
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07872021B2
反応ノート
読み込み中…