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Hydrochloric Acid → 3-(2,4-Difluorophenyl)sulfanylpropan-1-ol

HRID 600547
ノート
印刷プレビュー

反応式

HRID 600547 の反応式
Cl.[F:2][C:3]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:4]=1[S:10][CH2:11][CH2:12][CH2:13][O:14]C1CCCCO1>CO>[F:2][C:3]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:4]=1[S:10][CH2:11][CH2:12][CH2:13][OH:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 576632252-[3-(2,4-Difluorophenyl)sulfanylpropoxy]oxane2 回

生成物 1

HCID 433923683-(2,4-Difluorophenyl)sulfanylpropan-1-ol収率 99.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1M Hydrochloric acid (170 mL) was added to a solution of 2-[3-(2,4-difluorophenyl)sulfanylpropoxy]oxane (Intermediate 26) (10.8 g, 37 mmol) in methanol (170 mL) and stirred at ambient temperature for 40 minutes. The methanol was removed under reduced pressure and the remaining aqueous phase taken to pH 6. The solution was extracted with ethyl acetate (3×50 mL) and the combined organics washed with brine (50 mL), dried (MgSO4) and the solvent removed under reduced pressure to afford the product (7.5 g, 99%). 1H NMR δ (400 MHz, CDCl3): 1.38 (t, 1H), 1.83 (quintet, 2H), 2.97 (t, 2H), 3.77 (q, 2H), 6.81-6.87 (m, 2H), 7.38-7.45 (m, 1H).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customThe methanol was removed under reduced pressure
  2. extractionThe solution was extracted with ethyl acetate (3×50 mL)
  3. washthe combined organics washed with brine (50 mL)
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-7838517c257f43efac0eda19954ef813
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07902200B2

反応ノート

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