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

HRID 1607688노트

반응식

HRID 1607688 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]([O: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[O: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:12])=[O:13]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 164009FK 3311HCID 4311764Sodium borohydride

생성물 1

HCID 104501152'-(2,4-Difluorophenoxy)-4'-(1-hydroxyethyl)methanesulfonanilide수율 72%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium borohydride (0.18 g) was added portionwise to a solution of 4'-acetyl-2'-(2,4-difluorophenoxy)methanesulfonanilide (1.34 g) in methanol (25 ml) at room temperature. The mixture was stirred for 30 minutes, treated with acetic acid (1 ml), and concentrated under reduced pressure. The residue was dissolved in ethyl acetate, washed with an aqueous solution of sodium bicarbonate, and dried over magnesium sulfate. The ethyl acetate layer was evaporated to dryness and the residue was recrystallized from a mixture of ethanol and water to give pale yellow prisms of 2'-(2,4-difluorophenoxy)-4'-(1-hydroxyethyl)methanesulfonanilide (0.97 g).

후처리

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with an aqueous solution of sodium bicarbonate
  4. dry with materialdried over magnesium sulfate
  5. customThe ethyl acetate layer was evaporated to dryness
  6. customthe residue was recrystallized from a mixture of ethanol and water

출처 및 근거

ORD 기록
ord-96d5aad6da4847ceb9cffe7a535a1399
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04866091

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