Tert-Butylamine → N-tert-butyl-2-fluoro-4-methylbenzenesulfonamide

HRID 42335ノート

反応式

HRID 42335 の反応式
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].[F:6][C:7]1[CH:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:8]=1[S:14](Cl)(=[O:16])=[O:15]>C1COCC1>[C:1]([NH:5][S:14]([C:8]1[CH:9]=[CH:10][C:11]([CH3:13])=[CH:12][C:7]=1[F:6])(=[O:15])=[O:16])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 6385Tert-ButylamineHCID 27784822-Fluoro-4-methylbenzenesulphonyl chloride

生成物 1

HCID 11107608N-tert-butyl-2-fluoro-4-methylbenzenesulfonamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

To an ice cooled solution of tert-butylamine (12.55 ml) in THF (60 ml) was added a solution of 2-fluoro-4-methylbenzene-1-sulfonyl chloride (5 g) in THF (25 ml), dropwise. After stirring for 15 min at 0° C., the reaction mixture was allowed to warm and stirred at room temperature for 2 hours. The HCl salt was removed by filtration and the filtrate was concentrated to give a yellow residue, which was triturated with Et2O and Hexanes to give 5.10 g N-tert-butyl-2-fluoro-4-methylbenzenesulfonamide as an off-white granular solid.

後処理

  1. temperatureto warm
  2. stirringstirred at room temperature for 2 hours
  3. customThe HCl salt was removed by filtration
  4. concentrationthe filtrate was concentrated
  5. customto give a yellow residue, which
  6. customwas triturated with Et2O and Hexanes

出典と根拠

ORDレコード
ord-a7424409105145a4ae3d3ec5c4cf105f
出典データセット
uspto-grants-2013_09
特許番号
US08536187B2

反応ノート

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