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

HRID 484094
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HRID 484094 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c9f7af39bb564179bb03fb87037d5eb9
출처 데이터셋
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05229403

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