Sodium Hydroxide → 5-Carboxy-2-fluorobenzenesulfinic acid

HRID 33782

반응식

HRID 33782 반응식
S([O-])([O-])=O.[Na+].[Na+].Cl[S:8]([C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][C:19]=1[F:20])[C:14]([OH:16])=[O:15])(=[O:10])=[O:9].[OH-].[Na+]>O>[F:20][C:19]1[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[CH:12][C:11]=1[S:8]([OH:10])=[O:9]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24437Sodium SulfiteHCID 39298913-(Chlorosulfonyl)-4-fluorobenzoic acid

생성물 1

HCID 106796785-Carboxy-2-fluorobenzenesulfinic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Sodium sulphite (130 g, 1.034 mol) was added slowly to a solution of 3-chlorosulfonyl-4-fluoro-benzoic acid (49.39 g, 0.207 mol) in water (150 ml) at 0° C. with a vigorous stirring. After the addition was completed the reaction was warmed back to room temperature for 1 hour and the pH of the solution was kept around pH 6-7 with 2N sodium hydroxide solution. The white milky suspension was filtered and the solid washed with 2N sodium hydroxide solution (150 ml) and then water (100 ml). The filtrate was then cooled in an ice bath and concentrated HCl was added until no more precipitate was formed (pH<1). The white precipitate was then filtered, pressed dry and left in a dessicator overnight under vacuum and over activated silica (27.92 g, 66%). m/z (LC-MS, ESP), RT=0.98 min, (M−−1)=203

후처리

  1. additionAfter the addition
  2. filtrationThe white milky suspension was filtered
  3. washthe solid washed with 2N sodium hydroxide solution (150 ml)
  4. temperatureThe filtrate was then cooled in an ice bath
  5. additionconcentrated HCl was added until no more precipitate
  6. customwas formed (pH<1)
  7. filtrationThe white precipitate was then filtered
  8. custompressed dry

출처 및 근거

ORD 기록
ord-05a57145ebb44160bc662e6725e60535
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429660B2

연결된 노트

불러오는 중…