Hydrochloric Acid → 2,4-Dichloro-5-carboxybenzenesulfinic acid

HRID 1606597노트

반응식

HRID 1606597 반응식
S([O-])([O-])=O.[Na+].[Na+].[Cl:7][C:8]1[CH:16]=[C:15]([Cl:17])[C:14]([S:18](Cl)(=[O:20])=[O:19])=[CH:13][C:9]=1[C:10]([OH:12])=[O:11].[OH-].[Na+].Cl>O>[Cl:17][C:15]1[CH:16]=[C:8]([Cl:7])[C:9]([C:10]([OH:12])=[O:11])=[CH:13][C:14]=1[S:18]([OH:20])=[O:19]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 24437Sodium SulfiteHCID 773362,4-Dichloro-5-(chlorosulphonyl)benzoic acid

생성물 1

HCID 215439462,4-Dichloro-5-carboxybenzenesulfinic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
25 °C

실험 절차

A three liter flask equipped with a mechanical stirrer, thermometer and dropping funnel is charged with sodium sulfite (378 g,; 3.0 moles) and water (1 liter). The solution is cooled in an ice bath and treated with 2,4-dichloro-5-chlorosulfonylbenzoic acid (290 g.; 1.0 mole) and 10N sodium hydroxide (290 ml.) simultaneously in small portions over a period of 1.5 hours keeping the temperature below 20° C. and the pH of the reaction at 9. When the addition of the reagents is complete, the reaction is stirred for 3 hours at 25° C. then cooled to 10° C. and acidified with concentrated hydrochloric acid (440 ml.). The 2,4-dichloro-5-carboxybenzenesulfinic acid which precipitates is filtered, washed with ice water, then used in the next step without further purification.

후처리

  1. customA three liter flask equipped with a mechanical stirrer
  2. temperatureThe solution is cooled in an ice bath
  3. customthe temperature below 20° C.
  4. customthe pH of the reaction at 9
  5. additionWhen the addition of the reagents
  6. temperaturethen cooled to 10° C.
  7. customThe 2,4-dichloro-5-carboxybenzenesulfinic acid which precipitates
  8. filtrationis filtered
  9. washwashed with ice water
  10. customused in the next step without further purification

출처 및 근거

ORD 기록
ord-bb61811a6f2743e6924213fbc8dc8097
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03953476

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