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

HRID 20554

反応式

HRID 20554 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
150 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-e9d217611dd942d58da602e9cc758320
出典データセット
uspto-grants-2010_06
特許番号
US07745475B2

関連ノート

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