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Triethylamine → 3-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]-benzenesulfonic acid-[2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-N-methylethylamide]

HRID 654019
ノート
印刷プレビュー

反応式

HRID 654019 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][S:9]([C:12]2[CH:13]=[C:14]([S:18](Cl)(=[O:20])=[O:19])[CH:15]=[CH:16][CH:17]=2)(=[O:11])=[O:10])=[C:4]([C:22]([F:25])([F:24])[F:23])[CH:3]=1.C(N(CC)CC)C.[OH:33][CH:34]([CH:38]1[CH2:42][O:41][C:40]([CH3:44])([CH3:43])[O:39]1)[CH2:35][NH:36][CH3:37]>O1CCCC1>[OH:33][CH:34]([CH:38]1[CH2:42][O:41][C:40]([CH3:44])([CH3:43])[O:39]1)[CH2:35][N:36]([CH3:37])[S:18]([C:14]1[CH:15]=[CH:16][CH:17]=[C:12]([S:9](=[O:11])(=[O:10])[NH:8][C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][C:4]=2[C:22]([F:25])([F:24])[F:23])[CH:13]=1)(=[O:20])=[O:19]
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 3

HCID 8471TriethylamineHCID 150576173-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]-benzenesulfonic acid chlorideHCID 150576531-(2,2-Dimethyl-1,3-dioxolan-4-yl)-2-(methylamino)ethan-1-ol

生成物 1

HCID 678998783-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]-benzenesulfonic acid-[2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-N-methylethylamide]

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
45 °C

実験手順

8.36 g (20 mmol) of 3-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]-benzenesulfonic acid chloride is dissolved in 40 ml of tetrahydrofuran, 2.52 g (25 mmol) of triethylamine and 4.03 (25 mmol) of 2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-N-methylethylamine are added and stirred for 3 hours at 45° C. The reaction mixture is then concentrated by evaporation under reduced pressure, the residue is extracted with ethyl acetate and the extract is chromatographed on silica gel 60 (Merck) with ethyl acetate/hexane. 9.35 g (16.8 mmol)=84% of the theoretical yield is obtained as an amorphous solid.

後処理

  1. concentrationThe reaction mixture is then concentrated by evaporation under reduced pressure
  2. extractionthe residue is extracted with ethyl acetate
  3. customthe extract is chromatographed on silica gel 60 (Merck) with ethyl acetate/hexane
  4. custom9.35 g (16.8 mmol)=84% of the theoretical yield
  5. customis obtained as an amorphous solid

出典と根拠

ORDレコード
ord-a76d1f7cf3dc40a2aff7c1ef54e73eb8
出典データセット
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05130119

反応ノート

読み込み中…

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