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

HRID 1607688ノート

反応式

HRID 1607688 の反応式
[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]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 164009FK 3311HCID 4311764Sodium borohydride

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-96d5aad6da4847ceb9cffe7a535a1399
出典データセット
uspto-grants-1989_09
特許番号
US04866091

反応ノート

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