Tetrahydrofuran → HCID 178449877、化合物

HRID 570746ノート

反応式

HRID 570746 の反応式
[F:1][C:2]([F:13])([F:12])[CH2:3][O:4][C:5]1[CH:11]=[CH:10][C:8]([NH2:9])=[CH:7][CH:6]=1.C([N:16]([CH2:19][CH3:20])CC)C.[CH2:21]1COC[CH2:22]1.C(OCC)(=O)C>O>[F:1][C:2]([F:12])([F:13])[CH2:3][O:4][C:5]1[CH:11]=[CH:10][C:8]([NH:9][C:19](=[NH:16])[CH2:20][CH2:21][CH3:22])=[CH:7][CH:6]=1

参加物

6

反応条件

温度
70 °C

実験手順

A mixture of ethyl butylimidate hydrochloride (10.0 g), 4-(2,2,2-trifluoroethoxy)aniline (12.6 g), triethylamine (6.67 g) and THF (250 mL) was stirred at 70° C. for 2 days. To the reaction mixture were added ethyl acetate and water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to aminopropylsilane-bonded silica gel column chromatography (ethyl acetate/hexane) to give the title compound (4.80 g) as a solid.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-0af3bb64acb847fab8f831589a93f56d
出典データセット
uspto-grants-2015_05
特許番号
US09023858B2

反応ノート

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