Hydrazine hydrate (1:1) → HCID 58298858、化合物
反応式
O.[NH2:2][NH2:3].[CH2:4]([C:6]1[C:15]([CH3:16])=[C:14]([OH:17])[CH:13]=[CH:12][C:7]=1[C:8](OC)=[O:9])[CH3:5]>C(O)CCC>[CH2:4]([C:6]1[C:15]([CH3:16])=[C:14]([OH:17])[CH:13]=[CH:12][C:7]=1[C:8]([NH:2][NH2:3])=[O:9])[CH3:5]参加物
4
実験手順
1 ml of butanol and 4.5 ml of hydrazine hydrate are added to 1.88 g of methyl 2-ethyl-4-hydroxy-3-methylbenzoate in a screw-lid vial, and the mixture is stirred at 100° C. until the hydrazide formation is complete. The cooled reaction mixture is poured onto water, the precipitate is filtered off with suction and dried. Purification by recrystallisation from water/1 -propanol gives 1.28 g of 2-ethyl-4-hydroxy-3-methylbenzohydrazide as colourless crystals (68%); MS-FAB (M+H+)=1.95.1; Rf (polar method): 0.99 min.
後処理
- customThe cooled reaction mixture
- additionis poured onto water
- filtrationthe precipitate is filtered off with suction
- customdried
- customPurification
- customby recrystallisation from water/1 -propanol
出典と根拠
- ORDレコード
- ord-0716cc1de5504ae1a87d2fbc6fdb1aee
- 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…