反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[I:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][C:18]=1[O:19][CH2:20][CH2:21][C:22]1[CH:26]=[CH:25][S:24][CH:23]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)Cl>[I:12][C:13]1[CH:14]=[N+:15]([O-:9])[CH:16]=[CH:17][C:18]=1[O:19][CH2:20][CH2:21][C:22]1[CH:26]=[CH:25][S:24][CH:23]=1参加物
5
実験手順
m-Chloroperbenzoic acid (1.55 g, 6.29 mmol) was added portionwise to a solution of 1.0 g (3.02 mmol) of 3-iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine in 150 ml of methylene chloride. The mixture was stirred for 18 hours then mixed with 100 ml of 1 M aqueous sodium carbonate. The organic layer was separated and the aqueous one was extracted 2 times with 10 ml of methylene chloride. Combined organic extracts were washed with brine and dried over sodium sulfate. The solution was concentrated in vacuum to give 3-iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine 1-oxide (1.01 g, 92%). MS: (ESI+) 348.0
後処理
- customThe organic layer was separated
- extractionthe aqueous one was extracted 2 times with 10 ml of methylene chloride
- washCombined organic extracts were washed with brine
- dry with materialdried over sodium sulfate
- concentrationThe solution was concentrated in vacuum
出典と根拠
- ORDレコード
- ord-bb7485e41aca4e91974363d6d971d27c
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09309265B2
関連ノート
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