Carbon Dioxide → 5-Chloro-8-hydroxy-2-methyl-7-quinolinesulfonyl fluoride

HRID 382888

반응식

HRID 382888 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([CH3:13])=[N:7]2.C(=O)=O.[F:17][S:18](O)(=[O:20])=[O:19]>O>[Cl:1][C:2]1[CH:11]=[C:10]([S:18]([F:17])(=[O:20])=[O:19])[C:9]([OH:12])=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([CH3:13])=[N:7]2

참가 물질

5

반응물 3

HCID 280Carbon DioxideHCID 24603Fluorosulfuric acidHCID 129451955-Chloro-2-methylquinolin-8-ol

생성물 1

HCID 183725045-Chloro-8-hydroxy-2-methyl-7-quinolinesulfonyl fluoride

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
-78 °C

실험 절차

A solution of 5-chloro-8-hydroxy-2-methylquinoline (9.2 g) in 55 mL of fluorosulfonic acid is stirred at 120° C. for 18 h in a tightly stoppered flask. The mixture is then cooled to −78° C. and poured onto an intimate mixture of 250 mL of crushed ice and 250 mL of powdered dry ice. The mixture is allowed to warm to 25° C., and then diluted with distilled water until further addition causes no additional solid to precipitate (ca. 100 mL). The mixture is filtered, and the solid obtained is washed with four 50 mL-portions of 0° C. distilled water and then dried in a stream of air to give 10.7 g of the title compound as an orange powder.

후처리

  1. temperatureto warm to 25° C.
  2. customto precipitate (ca. 100 mL)
  3. filtrationThe mixture is filtered
  4. customthe solid obtained
  5. washis washed with four 50 mL-portions of 0° C.
  6. distillationdistilled water
  7. customdried in a stream of air

출처 및 근거

ORD 기록
ord-31877132c7974229bb46c8fb004512d3
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06310211B1

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