Methanol → 6-Azidohex-1-yne
反応式
S(OCCCCC#C)([C:4]1[CH:10]=[CH:9][C:7](C)=[CH:6][CH:5]=1)(=O)=O.[N-:18]=[N+:19]=[N-:20].[Na+].CO>O>[N:18]([CH2:10][CH2:9][CH2:7][CH2:6][C:5]#[CH:4])=[N+:19]=[N-:20]参加物
5
実験手順
A mixture containing 0.397 mole of hex-5-yn-1-ol tosylate; 0.76 mole of sodium azide; and one liter of methanol and 200 ml. of water is stirred at 60° C for 4 hours. The mixture is then evaporated under vacuum to remove the majority of the methanol and the remaining concentrate then poured into 500 ml. of ethyl ether, and then extracted three times with water, and dried over anhydrous magnesium sulfate and filtered. The filtrate is then evaporated, under vacuum, affording 1-azidohex-5-yne as a residue.
後処理
- customThe mixture is then evaporated under vacuum
- customto remove the majority of the methanol
- concentrationthe remaining concentrate
- additionthen poured into 500 ml
- extractionof ethyl ether, and then extracted three times with water
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customThe filtrate is then evaporated, under vacuum
出典と根拠
- ORDレコード
- ord-46cf7dadc21a466e980df03c36b439ac
- 出典データセット
- uspto-grants-1977_12
- 特許番号
- US04064257
反応ノート
読み込み中…