Triethylamine → HCID 22020971、化合物
反応式
[O:1]1[C:9]2[C:4](=[N:5][CH:6]=[CH:7][CH:8]=2)[O:3][CH:2]1[CH2:10][OH:11].C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>C(Cl)Cl>[CH3:19][S:20]([O:11][CH2:10][CH:2]1[O:3][C:4]2=[N:5][CH:6]=[CH:7][CH:8]=[C:9]2[O:1]1)(=[O:22])=[O:21]参加物
5
実験手順
A solution of intermediate (5) (0.018 mol) and triethyl amine (0.036 mol) in DCM (80 ml) was stirred and cooled with an ice-water bath. Methanesulfonyl chloride (0.027 mol) was added dropwise and the resulting reaction mixture was stirred for one hour while cooling on an ice-bath. The crude reaction mixture was washed with water and brine, then extracted. The separated organic layer was dried, filtered and the solvent was evaporated, yielding 4.2 g of (±)-1,3-dioxolo[4,5-b]pyridine-2-methanol methanesulfonate (ester) (intermediate 6).
後処理
- temperaturecooled with an ice-water bath
- customthe resulting reaction mixture
- temperaturewhile cooling on an ice-bath
- customThe crude reaction mixture
- washwas washed with water and brine
- extractionextracted
- customThe separated organic layer was dried
- filtrationfiltered
- customthe solvent was evaporated
出典と根拠
- ORDレコード
- ord-a094a34095174cc381d440ed23ac3e00
- 出典データセット
- uspto-grants-2006_07
- 特許番号
- US07081453B2
反応ノート
読み込み中…