Dimethylformamide → 4-(5-Amino-1,3,4-oxadiazol-2-yl)-3-ethyl-2-methylphenol
反応式
[N:1]#[C:2]Br.[CH2:4]([C:6]1[C:15]([CH3:16])=[C:14]([OH:17])[CH:13]=[CH:12][C:7]=1[C:8]([NH:10][NH2:11])=[O:9])[CH3:5].C(=O)([O-])O.[Na+].CN(C=O)C>O>[NH2:1][C:2]1[O:9][C:8]([C:7]2[CH:12]=[CH:13][C:14]([OH:17])=[C:15]([CH3:16])[C:6]=2[CH2:4][CH3:5])=[N:10][N:11]=1参加物
6
実験手順
196 mg of cyanogen bromide are added dropwise to a solution of 300 mg of 2-ethyl-4-hydroxy-3-methylbenzohydrazide in 50 ml of water, 130 mg of sodium hydrogencarbonate and 4 ml of DMF. A gas forms and a precipitate deposits. The latter is filtered off with suction and purified by column chromatography on silica gel, giving 40 mg of 4-(5-amino-1,3,4-oxadiazol-2-yl)-3-ethyl-2-methylphenol as colourless powder; MS-FAB (M+H+)=220; Rf (polar method): 1.43 min;
後処理
- filtrationThe latter is filtered off with suction
- custompurified by column chromatography on silica gel
出典と根拠
- ORDレコード
- ord-cca37965340a499c8b8cfb5de7a3c74d
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08377975B2
反応ノート
読み込み中…