Sodium Sulfite → Sodium benzoxazole-2-methanesulfonate

HRID 427088

반응식

HRID 427088 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

HCID 23672978Sodium benzoxazole-2-methanesulfonate수율 135.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-843070517e574e1dbf381502713159f3
출처 데이터셋
uspto-grants-1979_10
특허 번호
US04172896

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