Chlorosulfonic acid → HCID 178524660、化合物
反応式
[OH:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[Cl:11][S:12](O)(=[O:14])=[O:13]>>[Cl:11][S:12]([C:8]1[CH:9]=[N:10][C:2]([OH:1])=[C:3]([CH:7]=1)[C:4]([OH:6])=[O:5])(=[O:14])=[O:13]参加物
3
反応条件
- 温度
- 160 °C
実験手順
2-Hydroxynicotinic acid (10.0 g, 71.8 mmol) was dissolved in 25 ml of chlorosulfonic acid and heated to 160° C. overnight. After cooling the reaction was slowly poured into ice and stirred in an ice bath until a white precipitate formed. The solid was filtered off and dried under vacuum to afford 7.55 g of 5-(chlorosulfonyl)-2-hydroxynicotinic acid (44% yield). 1H NMR (300 MHz, DMSO-d6) δ ppm 7.9 (dd, J=2.5, 0.7 Hz, 1H) 8.4 (dd, J=2.6, 0.7 Hz, 1H).
後処理
- temperatureAfter cooling the reaction
- additionwas slowly poured into ice
- customformed
- filtrationThe solid was filtered off
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-7124389b873741a48a2103f353314827
- 出典データセット
- uspto-grants-2010_01
- 特許番号
- US07645771B2
反応ノート
読み込み中…