Potassium Carbonate → (5-(Difluoromethyl)furan-2-yl)methanol

HRID 560564ノート

反応式

HRID 560564 の反応式
C(=O)([O-])[O-].[K+].[K+].C([O:10][CH2:11][C:12]1[O:13][C:14]([CH:17]([F:19])[F:18])=[CH:15][CH:16]=1)(=O)C>CO>[F:18][CH:17]([F:19])[C:14]1[O:13][C:12]([CH2:11][OH:10])=[CH:16][CH:15]=1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 53728052(5-(Difluoromethyl)furan-2-yl)methyl acetate

生成物 1

HCID 20079677(5-(Difluoromethyl)furan-2-yl)methanol収率 96%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a suspension of potassium carbonate in anhydrous methanol (10%, 50 mL) was added (5-(difluoromethyl)furan-2-yl)methyl acetate (4.21 g, 22.16 mmol). The reaction mixture was stirred at ambient temperature for 20 minutes, filtered and concentrated in vacuo. The residue was purified by column chromatography eluted with ethyl acetate/hexane (3/7) to afford (5-(difluoromethyl)furan-2-yl)methanol as a yellow oil in 96% yield (3.15 g): 1H NMR (300 MHz, CDCl3) δ 6.55 (t, JH-F=54.2 Hz, 1H), 6.58-6.55 (m, 1H), 6.34-6.26 (m, 1H), 4.59 (d. J=5.9 Hz, 2H).

後処理

  1. filtrationfiltered
  2. concentrationconcentrated in vacuo
  3. customThe residue was purified by column chromatography
  4. washeluted with ethyl acetate/hexane (3/7)

出典と根拠

ORDレコード
ord-bc41e2476d0c4d1d91622ffa9a7097f9
出典データセット
uspto-grants-2011_11
特許番号
US08063084B2

反応ノート

読み込み中…