Thionyl Chloride → 4-Bromothiazole-2-carbohydrazide
反応式
[Br:1][C:2]1[N:3]=[C:4]([C:7]([OH:9])=O)[S:5][CH:6]=1.O=S(Cl)Cl.O.[NH2:15][NH2:16]>CO>[Br:1][C:2]1[N:3]=[C:4]([C:7]([NH:15][NH2:16])=[O:9])[S:5][CH:6]=1参加物
5
実験手順
To a solution of the 4-bromothiazole-2-carboxylic acid (2.0 g, 9.8 mmol) in MeOH (10 mL) was added SOCl2 (710 μL, 9.8 mmol) and the reaction was refluxed for 3 hours. The reaction was concentrated, the residue was suspended in EtOH (10 mL), hydrazine hydrate (2.4 mL, 49 mmol) was added and the reaction was heated to reflux for 90 minutes. The reaction was concentrated, suspended in CH3CN, filtered, and the solids were washed with CH3CN, Et2O, and dried to afford 1.7 g (77%) of 4-bromothiazole-2-carbohydrazide as a yellow solid. M+1=222.1
後処理
- temperaturethe reaction was refluxed for 3 hours
- concentrationThe reaction was concentrated
- temperaturethe reaction was heated
- temperatureto reflux for 90 minutes
- concentrationThe reaction was concentrated
- filtrationfiltered
- washthe solids were washed with CH3CN, Et2O
- customdried
出典と根拠
- ORDレコード
- ord-0a18f912c896420fa0b5841ba0777e66
- 出典データセット
- uspto-grants-2015_06
- 特許番号
- US09051313B2
反応ノート
読み込み中…