Piperazine → 2-(Piperazin-1-yl)-1,3-thiazole-5-carboxylic acid
反応式
Br[C:2]1(C(O)=O)[NH:6][CH:5]=[CH:4][S:3]1.[NH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.[C:16]([O-])([O-:18])=[O:17].[K+].[K+]>O1CCOCC1>[N:10]1([C:2]2[S:3][C:4]([C:16]([OH:18])=[O:17])=[CH:5][N:6]=2)[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1参加物
5
実験手順
2-Bromothiazole carboxylic acid 1 (1 g; 4.8 mmol) and piperazine (6.2 g; 72 mmol; 24 equiv.) were dissolved in dioxane, K2CO3 (3.32 g; 24 mmol; 5 equiv.) was added and the suspension was refluxed over night. The solvent was removed at the rotary evaporator, the residue dissolved in ethanol, filtered and recrystallized. The crude product was dried at the oil pump and directly used in the following step.
後処理
- temperaturethe suspension was refluxed over night
- customThe solvent was removed at the rotary evaporator
- dissolutionthe residue dissolved in ethanol
- filtrationfiltered
- customrecrystallized
- dry with materialThe crude product was dried at the oil pump
出典と根拠
- ORDレコード
- ord-540876f9926548bb87ef494dd0757107
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846682B2
反応ノート
読み込み中…