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Acetic Acid → 2'-(2,4-Difluorophenylamino)-4'-(1-hydroxyethyl)methanesulfonanilide

HRID 1087209
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반응식

HRID 1087209 반응식
[BH4-].[Na+].[C:3]([C:6]1[CH:16]=[CH:15][C:9]([NH:10][S:11]([CH3:14])(=[O:13])=[O:12])=[C:8]([NH:17][C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:19]=2[F:25])[CH:7]=1)(=[O:5])[CH3:4].C(O)(=O)C>CO>[F:25][C:19]1[CH:20]=[C:21]([F:24])[CH:22]=[CH:23][C:18]=1[NH:17][C:8]1[CH:7]=[C:6]([CH:3]([OH:5])[CH3:4])[CH:16]=[CH:15][C:9]=1[NH:10][S:11]([CH3:14])(=[O:13])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 4311764Sodium borohydrideHCID 10472404HCID 10472404, 화합물

생성물 1

HCID 198177352'-(2,4-Difluorophenylamino)-4'-(1-hydroxyethyl)methanesulfonanilide수율 59%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium borohydride (0.2 g) was added portionwise to a solution of 4'-acetyl-2'-(2,4-difluorophenylamino)methanesulfonanilide (1.5 g) in methanol (15 ml) at 5° to 10° C. The mixture was stirred for 10 hours at room temperature, treated with acetic acid, and concentrated. The residue was triturated with water and filtered. The solid (1.6 g) was recrystallized from a mixture of ethanol and ethyl acetate to give colorless needles of 2'-(2,4-difluorophenylamino)-4'-(1-hydroxyethyl)methanesulfonanilide (0.89 g).

후처리

  1. concentrationconcentrated
  2. customThe residue was triturated with water
  3. filtrationfiltered
  4. customThe solid (1.6 g) was recrystallized from a mixture of ethanol and ethyl acetate

출처 및 근거

ORD 기록
ord-c6c7c42167474d90a4a3265dfdc17545
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05034417

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