Sulfuric Acid → HCID 14249478、化合物
反応式
[N:1]([CH2:4][CH:5]([OH:10])[CH:6]([OH:9])[CH2:7][OH:8])=[N+:2]=[N-:3].CO[C:13](OC)([CH3:15])[CH3:14].S(=O)(=O)(O)O.[OH-].[Na+]>CC(C)=O>[N:1]([CH2:4][CH:5]([CH:6]1[CH2:7][O:8][C:13]([CH3:15])([CH3:14])[O:9]1)[OH:10])=[N+:2]=[N-:3]参加物
6
実験手順
A solution of 14.71 g of 4-azido-1,2,3-butanetriol in 30 ml of acetone is combined with 13.95 g of 2,2-dimethoxypropane, as well as 0.1 ml of concentrated sulfuric acid. The mixture is stirred overnight at room temperature, neutralized with 2N sodium hydroxide solution, and concentrated to dryness under vacuum. The residue is distilled with a water-jet aspirator. 2-Azido-(2,2-dimethyl-1,3-dioxolan-4-yl)ethanol passes over as a colorless oil at 130°-132° C./13 mm. Yield: 11.79 g (63% of theory).
後処理
- concentrationconcentrated to dryness under vacuum
- distillationThe residue is distilled with a water-jet aspirator
- custompasses over as a colorless oil at 130°-132° C.
出典と根拠
- ORDレコード
- ord-c4275ce7288846a694b086c6e9121113
- 出典データセット
- uspto-grants-1986_02
- 特許番号
- US04570007
反応ノート
読み込み中…