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

HRID 33783

反応式

HRID 33783 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
140 °C

実験手順

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.

後処理

  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%)

出典と根拠

ORDレコード
ord-667e20ec9f2246dd8df81440fb1cb236
出典データセット
uspto-grants-2008_09
特許番号
US07429660B2

関連ノート

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