Bromoacetic Acid → 1,2,4-Trifluoro-5-(methylsulfonyl)benzene

HRID 20554

반응식

HRID 20554 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[S:10](Cl)(=[O:12])=[O:11].S([O-])([O-])=O.[Na+].[Na+].[C:20](=O)(O)[O-].[Na+].BrCC(O)=O>O>[F:9][C:5]1[CH:4]=[C:3]([S:10]([CH3:20])(=[O:12])=[O:11])[C:2]([F:1])=[CH:7][C:6]=1[F:8]

참가 물질

6

반응물 4

HCID 6227Bromoacetic AcidHCID 24437Sodium SulfiteHCID 516892Sodium BicarbonateHCID 27769792,4,5-Trifluorobenzenesulfonyl chloride

생성물 1

HCID 467393961,2,4-Trifluoro-5-(methylsulfonyl)benzene수율 66.5%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
150 °C

실험 절차

2,4,5-Trifluorophenyl sulfonyl chloride (279 mg) was added to a solution of sodium sulfite (306 mg) and sodium bicarbonate (153 mg) in water (4 mL). The mixture was heated to 150° C. in a sealed microwave vial for 400 seconds and allowed to cool. The mixture was treated with bromoacetic acid (253 mg) in water (1 mL), and heated to 150° C. for 300 seconds then allowed to cool, following which the precipitate was removed by filtration and dried in vacuo to give the desired compound (169 mg). The material was used without further purification. 1H NMR δ (d6-DMSO): 3.35 (s, 3H), 7.87-8.01 (m, 2H).

후처리

  1. temperatureto cool
  2. temperatureheated to 150° C. for 300 seconds
  3. temperatureto cool
  4. customwas removed by filtration
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-e9d217611dd942d58da602e9cc758320
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745475B2

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