Sodium Hydroxide → 4-(2-Bromo-phenylsulfanyl)-3-sulfino-benzoic Acid

HRID 33783

반응식

HRID 33783 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[SH:8].F[C:10]1[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[CH:12][C:11]=1[S:19]([OH:21])=[O:20].[OH-].[Na+]>O>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][C:10]1[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[CH:12][C:11]=1[S:19]([OH:21])=[O:20]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 805982-BromobenzenethiolHCID 106796785-Carboxy-2-fluorobenzenesulfinic acid

생성물 1

HCID 221394104-(2-Bromo-phenylsulfanyl)-3-sulfino-benzoic Acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
140 °C

실험 절차

2-Bromobenzenethiol (25 g, 132 mmol) was added to a solution of 4-fluoro-3-sulfino-benzoic acid (13.5 g, 66 mmol) and NaOH pellets (11 g, 264 mmol) in water (30 ml). The yellow mixture was then degassed for 10 minutes and then heated to 140° C. for 48 hours. The reaction was then cooled to 0° C. and acidified to pH 4-5 (pH paper) with concentrated HCl. The precipitate formed was filtered, washed with hexane and was dried in a vacuum dessicator over activated silica overnight (20.69 g, 84%). m/z (LC-MS, ESP), RT=3.67 min, M−−1)=373.

후처리

  1. customThe yellow mixture was then degassed for 10 minutes
  2. temperatureThe reaction was then cooled to 0° C.
  3. customThe precipitate formed
  4. filtrationwas filtered
  5. washwashed with hexane
  6. customwas dried in a vacuum dessicator over activated silica overnight (20.69 g, 84%)

출처 및 근거

ORD 기록
ord-667e20ec9f2246dd8df81440fb1cb236
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429660B2

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