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Dimethylamine → HCID 20299643、化合物

HRID 1733471
ノート
印刷プレビュー

反応式

HRID 1733471 の反応式
[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[N:6]([CH:8]=[CH:9][N:10]=2)[CH:7]=1.S(Cl)(Cl)=O.[CH3:15][NH:16][CH3:17].Cl[S:19](O)(=[O:21])=[O:20]>>[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[N:6]([C:8]([S:19](=[O:21])(=[O:20])[N:16]([CH3:17])[CH3:15])=[CH:9][N:10]=2)[CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 674DimethylamineHCID 24386Thionyl ChlorideHCID 24638Chlorosulfonic acidHCID 128415726-Chloroimidazo[1,2-a]pyrazine

生成物 1

HCID 20299643HCID 20299643、化合物

反応条件

温度
100 °C

実験手順

6-Chloroimidazo[1,2-a]pyrazine (3.07 g, 0.020 mole) is added in portions with stirring to 20 ml chlorosulfonic acid, and the mixture heated 2 hours at 100° C. and then cooled to room temperature. Thionyl chloride (2 g) is added and the mixture reheated to 100° C. for 2 hours. After cooling to room temperature, the mixture is quenched on crushed ice and extracted with ether. The ether layer is dried over sodium sulfate, filtered and concentrated under vacuum to give an oil which is stirred with a mixture of crushed ice and aqueous dimethylamine for one hour. The crude 6-chloro-3-(N,N-dimethylsulfamoyl)imidazo[1,2-a]pyrazine is collected by filtration.

後処理

  1. temperaturecooled to room temperature
  2. temperatureAfter cooling to room temperature
  3. customthe mixture is quenched
  4. customon crushed ice
  5. extractionextracted with ether
  6. dry with materialThe ether layer is dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum
  9. customto give an oil which
  10. filtrationThe crude 6-chloro-3-(N,N-dimethylsulfamoyl)imidazo[1,2-a]pyrazine is collected by filtration

出典と根拠

ORDレコード
ord-7c3a96f302614c9393b0c6b60f716485
出典データセット
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04242344

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート