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2-(Dimethylsulfamoyl)benzene-1-sulfonyl isocyanate → 2-[[(4-Fluoro-6-trifluoromethoxypyrimidin-2-yl)aminocarbonyl]aminosulfonyl]benzenesulfonic acid N,N-dimethylamide

HRID 232529
ノート
印刷プレビュー

反応式

HRID 232529 の反応式
[CH3:1][N:2]([CH3:18])[S:3]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[S:12]([N:15]=[C:16]=[O:17])(=[O:14])=[O:13])(=[O:5])=[O:4].[NH2:19][C:20]1[N:25]=[C:24]([F:26])[CH:23]=[C:22]([O:27][C:28]([F:31])([F:30])[F:29])[N:21]=1>C(Cl)Cl>[CH3:1][N:2]([CH3:18])[S:3]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[S:12]([NH:15][C:16]([NH:19][C:20]1[N:25]=[C:24]([F:26])[CH:23]=[C:22]([O:27][C:28]([F:30])([F:31])[F:29])[N:21]=1)=[O:17])(=[O:13])=[O:14])(=[O:4])=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 133926792-(Dimethylsulfamoyl)benzene-1-sulfonyl isocyanateHCID 150227162-Amino-4-fluoro-6-trifluoromethoxypyrimidine

生成物 1

HCID 231784442-[[(4-Fluoro-6-trifluoromethoxypyrimidin-2-yl)aminocarbonyl]aminosulfonyl]benzenesulfonic acid N,N-dimethylamide収率 22%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5.9 g (20 mmol) of 2-(dimethylamino)sulfonylbenzenesulfonyl isocyanate were added to a solution of 4.0 g (20 mmol) of 2-amino-4-fluoro-6-trifluoromethoxypyrimidine in 30 ml of methylene chloride at 25° C. Stirring was carried out for 16 hours at 25° C., and the product which separated out was filtered off under suction, washed with a little ether and dried at 50° C. under reduced pressure from a water pump. 2.1 g of the title compound (22% of theory) of melting point 167°-169° C. were obtained in this manner. Further product can be isolated from the mother liquor.

後処理

  1. customthe product which separated out
  2. filtrationwas filtered off under suction
  3. washwashed with a little ether
  4. dry with materialdried at 50° C. under reduced pressure from a water pump

出典と根拠

ORDレコード
ord-911512e5eaee41d1843e677e474443d5
出典データセット
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05591694

反応ノート

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