Methanesulfonic Acid → HCID 20458166、化合物

HRID 544538ノート

反応式

HRID 544538 の反応式
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([S:14]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=2)=O)=[CH:10][CH:9]=1>C1(OC)C=CC=CC=1>[CH3:1][S:2]([O-:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([S+:14]([C:11]2[CH:12]=[CH:13][C:8]([O:7][CH3:6])=[CH:9][CH:10]=2)[C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=2)=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 238614Bis(4-methoxyphenyl) sulfoxide

生成物 1

HCID 20458166HCID 20458166、化合物収率 227.1%

試薬・触媒・溶媒 1

HCID 7519Anisole溶媒

反応条件

温度
80 °C

実験手順

A mixture of 192.22 g of methane sulfonic acid, 54.46 g of bis-(4-methoxyphenyl)sulfoxide and 500 ml of anisole was heated at 80° C. for 22 hours. The mixture was poured into 1000 g of ice water and extracted three times with 500-ml portions of ether. The aqueous phase was neutralized with 50 percent aqueous sodium hydroxide and extracted five times with 500-ml portions of chloroform. The combined chloroform phases were dried with magnesium sulfate and the chloroform was removed on a rotary evaporator to give 105.76 g of tris-(4-methoxyphenyl)sulfonium methane sulfonate with residual chloroform of solvation.

後処理

  1. extractionextracted three times with 500-ml portions of ether
  2. extractionextracted five times with 500-ml portions of chloroform
  3. dry with materialThe combined chloroform phases were dried with magnesium sulfate
  4. customthe chloroform was removed on a rotary evaporator

出典と根拠

ORDレコード
ord-9837f098476d4dcfa49690c934c1cdc1
出典データセット
uspto-grants-1984_05
特許番号
US04451409

反応ノート

読み込み中…