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

HRID 1992073노트

반응식

HRID 1992073 반응식
[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]

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178524660HCID 178524660, 화합물

생성물 1

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

반응 조건

온도
130 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-63dcb4723f3544288a60808636bcfd50
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07645771B2

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