Sodium Sulfite → Sodium benzoxazole-2-methanesulfonate

HRID 427088

反応式

HRID 427088 の反応式
Br[CH2:2][C:3]1[O:4][C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=1.[S:12]([O-:15])([O-:14])=[O:13].[Na+:16].[Na+]>CO.O>[O:4]1[C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=[C:3]1[CH2:2][S:12]([O-:15])(=[O:14])=[O:13].[Na+:16]

参加物

5

反応物 2

HCID 24437Sodium SulfiteHCID 127459442-(Bromomethyl)benzo[d]oxazole

生成物 1

HCID 23672978Sodium benzoxazole-2-methanesulfonate収率 135.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

To a solution of 3.0 g of 2-bromomethylbenzoxazole [prepared according to the procedures described in Belgian Pat. No. 624,463] in 40 ml of methanol was added a solution of 1.9 g of sodium sulfite in 40 ml of water. The mixture was heated with stirring at 60° C. for 6 hours and concentrated under reduced pressure to give crude sodium benzoxazole-2-methanesulfonate (4.5 g). To the sodium salt was added 15 ml of phosphorus oxychloride and the mixture was heated under reflux for one hour. The removal of the remaining phosphorus oxychloride by distillation under reduced pressure gave the desired product as an oil.

後処理

  1. temperatureThe mixture was heated
  2. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-843070517e574e1dbf381502713159f3
出典データセット
uspto-grants-1979_10
特許番号
US04172896

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