Triethylamine → 7-Methylsulfonyloxymethylbenzo-1,2,3-thiadiazole

HRID 257130

反応式

HRID 257130 の反応式
[OH:1][CH2:2][C:3]1[C:11]2[S:10][N:9]=[N:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:19][S:20]([O:1][CH2:2][C:3]1[C:11]2[S:10][N:9]=[N:8][C:7]=2[CH:6]=[CH:5][CH:4]=1)(=[O:22])=[O:21]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 200964331,2,3-Benzothiadiazol-7-ylmethanol

生成物 1

HCID 200964567-Methylsulfonyloxymethylbenzo-1,2,3-thiadiazole

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 3.32 g of 7-hydroxymethylbenzo-1,2,3-thiadiazole, 3.1 ml of triethylamine and 0.2 g of 4-dimethylaminopyridine in 50 ml of methylene chloride there is added dropwise with cooling at -5° to 0° C. a solution of 2.23 g of methanesulfonyl chloride in 15 ml of dichloromethane, and the mixture is stirred for 2 hours at room temperature. The reaction mixture is then treated with ice-water and extracted several times using dichloromethane. The combined extracts are washed with water, dried and evaporated. Chromatographic purification on silica gel (CH2Cl2) gives the title compound as a viscous resin.

後処理

  1. extractionextracted several times
  2. washThe combined extracts are washed with water
  3. customdried
  4. customevaporated
  5. customChromatographic purification on silica gel (CH2Cl2)

出典と根拠

ORDレコード
ord-d3bf367c5b404175b43a123d4f5cba0a
出典データセット
uspto-grants-1993_11
特許番号
US05260423

関連ノート

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