Formaldehyde → 6-(Hydroxymethyl)-2-methylpyridin-3-ol
反応式
[OH:1][C:2]1[C:3]([CH3:8])=[N:4][CH:5]=[CH:6][CH:7]=1.[OH-:9].[Na+].O.[CH2:12]=O>C(O)(=O)C>[OH:1][C:2]1[C:3]([CH3:8])=[N:4][C:5]([CH2:12][OH:9])=[CH:6][CH:7]=1参加物
6
実験手順
A mixture of 27.2 g. (0.25 mol) of 3-hydroxy-2-methylpyridine, 100 ml. of 10% sodium hydroxide in 75 ml. of water and 22.5 ml. (0.25 mol) of 40% formalin (aqueous methanolic formaldehyde solution) is refluxed for two hours. An additional amount of 40% formalin (22.5 ml.) is added and the reflux is continued for two hours. The mixture is acidified with acetic acid and the resulting precipitate is filtered and washed with acetone. The filtrate is evaporated to dryness and the residue is repeatedly extracted with hot acetone. The extract is dried, treated with charcoal and evaporated to give crude 3-hydroxy-6-hydroxymethyl-2-methylpyridine as a solid.
後処理
- additionA mixture of 27.2 g
- filtrationthe resulting precipitate is filtered
- washwashed with acetone
- customThe filtrate is evaporated to dryness
- extractionthe residue is repeatedly extracted with hot acetone
- customThe extract is dried
- additiontreated with charcoal
- customevaporated
出典と根拠
- ORDレコード
- ord-c2ac2dd992a4428c984cfc99a93c0289
- 出典データセット
- uspto-grants-1976_04
- 特許番号
- US03952101
反応ノート
読み込み中…