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Sodium Chloride → N-(3-amino-5-trifluoromethyl-2-pyridyl)ethanesulfonamide

HRID 484094
ノート
印刷プレビュー

反応式

HRID 484094 の反応式
S(S([O-])=O)([O-])=O.[Na+].[Na+].[N+:9]([C:12]1[C:13]([NH:22][S:23]([CH2:26][CH3:27])(=[O:25])=[O:24])=[N:14][CH:15]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:17]=1)([O-])=O.[Cl-].[Na+]>O.O1CCCC1>[NH2:9][C:12]1[C:13]([NH:22][S:23]([CH2:26][CH3:27])(=[O:25])=[O:24])=[N:14][CH:15]=[C:16]([C:18]([F:21])([F:19])[F:20])[CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 5234Sodium ChlorideHCID 24489Sodium DithioniteHCID 10851681N-(3-nitro-5-trifluoromethyl-2-pyridyl)ethanesulfonamide

生成物 1

HCID 10730665N-(3-amino-5-trifluoromethyl-2-pyridyl)ethanesulfonamide収率 93.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

An alternative process will be described. To a solution prepared by dissolving 34.9 g of sodium hydrosulfite in 400 ml of water, a solution prepared by dissolving 5.0 g of N-(3-nitro-5-trifluoromethyl-2-pyridyl)ethanesulfonamide in 80 ml of tetrahydrofuran, was dropwise added at room temperature. After completion of the dropwise addition, the mixture was reacted for further 3 hours. After completion of the reaction, sodium chloride was added until the tetrahydrofuran layer was separated. The separated tetrahydrofuran layer was dried, and tetrahydrofuran was distilled off under reduced pressure to obtain 4.2 g of N-(3-amino-5-trifluoromethyl-2-pyridyl)ethanesulfonamide.

後処理

  1. customTo a solution prepared
  2. customa solution prepared
  3. additionwas dropwise added at room temperature
  4. additionAfter completion of the dropwise addition
  5. customthe mixture was reacted for further 3 hours
  6. customwas separated
  7. dry with materialThe separated tetrahydrofuran layer was dried
  8. distillationtetrahydrofuran was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-c9f7af39bb564179bb03fb87037d5eb9
出典データセット
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05229403

反応ノート

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