Phosphorus oxychloride → 2-Chloro-5-(chlorosulfonyl)pyridine-3-carboxylic acid

HRID 1992073ノート

反応式

HRID 1992073 の反応式
[Cl:1][S:2]([C:5]1[CH:6]=[N:7][C:8](O)=[C:9]([CH:13]=1)[C:10]([OH:12])=[O:11])(=[O:4])=[O:3].O=P(Cl)(Cl)[Cl:17]>>[Cl:17][C:8]1[N:7]=[CH:6][C:5]([S:2]([Cl:1])(=[O:4])=[O:3])=[CH:13][C:9]=1[C:10]([OH:12])=[O:11]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178524660HCID 178524660、化合物

生成物 1

HCID 574159692-Chloro-5-(chlorosulfonyl)pyridine-3-carboxylic acid

反応条件

温度
130 °C

実験手順

5-(Chlorosulfonyl)-2-hydroxynicotinic acid (500 mg, 2.10 mmol) vas suspended in 5 ml of POCl3 in a sealed tube and heated to 130° C. until all solid had dissolved. The reaction was cooled to 0° C. and poured onto ice and stirred until a solid formed. The filtered white solid was dried to afford 2-chloro-5-(chlorosulfonyl)nicotinic acid. 1H NMR (400 MHz, Acetone-d6) δ ppm 8.9 (d, J=2.6 Hz, 10H), 9.3 (d, J=2.6 Hz, 10H).

後処理

  1. dissolutionhad dissolved
  2. temperatureThe reaction was cooled to 0° C.
  3. additionpoured onto ice
  4. customformed
  5. customThe filtered white solid was dried

出典と根拠

ORDレコード
ord-63dcb4723f3544288a60808636bcfd50
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…