Water → 4-(Azidomethyl)-2-thiazolamine
反応式
Cl[CH2:2][C:3]1[N:4]=[C:5]([NH2:8])[S:6][CH:7]=1.O.[N-:10]=[N+:11]=[N-:12].[Na+]>O1CCOCC1>[N:10]([CH2:2][C:3]1[N:4]=[C:5]([NH2:8])[S:6][CH:7]=1)=[N+:11]=[N-:12]参加物
5
実験手順
To a solution of 4-chloromethyl-thiazol-2-ylamine (7.45 g, 50.0 mmol) in dioxane:water mixture (8:2) was added sodium azide (4.87 g, 75.0 mmol) and the reaction mixture was refluxed for 2–3 h. The mixture was concentrated in vacuo to remove all dioxane and the residue was dissolved in EtOAc (200 mL). The organic layer was washed with water (2×200 mL), brine (2×200 mL), dried over (Na2SO4) and concentrated in vacuo to give 4-azidomethyl-thiazol-2-ylamine in 70–90% yield.
後処理
- temperaturethe reaction mixture was refluxed for 2–3 h
- concentrationThe mixture was concentrated in vacuo
- customto remove all dioxane
- dissolutionthe residue was dissolved in EtOAc (200 mL)
- washThe organic layer was washed with water (2×200 mL), brine (2×200 mL)
- dry with materialdried over (Na2SO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-682e7436e7f94a988d8ac2be814ac265
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07384967B2
反応ノート
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