Water → HCID 22005233、化合物

HRID 1681246ノート

反応式

HRID 1681246 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([C:14](OC)=[O:15])=[C:12]([CH3:18])[N:11]=[C:10]([CH:19]([CH3:21])[CH3:20])[C:9]=2[C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:4][CH:3]=1.O>C1(C)C=CC=CC=1.O1CCCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:13]([CH2:14][OH:15])=[C:12]([CH3:18])[N:11]=[C:10]([CH:19]([CH3:20])[CH3:21])[C:9]=2[C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 962WaterHCID 10155368HCID 10155368、化合物

生成物 1

HCID 22005233HCID 22005233、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

26.5 ml (92.75 mmol) of a 3.5 molar solution of sodium bis-(2-methoxyethoxy)-dihydroaluminate in toluene are added under nitrogen to a solution of 9.5 g (26.5 mmol) of the compound from Example 19 in 200 ml of absolute tetrahydrofuran at 0° C. and the mixture is stirred for 30 minutes at room temperature. After cooling again to 0° C., 200 ml of water are cautiously added dropwise and the mixture is extracted three times using 150 ml of ethyl acetate each time. The combined organic phases are washed once with saturated sodium chloride solution, dried over magnesium sulphate and concentrated in vacuo. The residue is chromatographed on a column (200 g of silica gel 70-230 mesh, φ4.5 cm, using ethyl acetate/petroleum ether 2:8).

後処理

  1. temperatureAfter cooling again to 0° C.
  2. extractionthe mixture is extracted three times
  3. washThe combined organic phases are washed once with saturated sodium chloride solution
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated in vacuo
  6. customThe residue is chromatographed on a column (200 g of silica gel 70-230 mesh, φ4.5 cm, using ethyl acetate/petroleum ether 2:8)

出典と根拠

ORDレコード
ord-9e12f42415214f3f8f9acab42a21cf13
出典データセット
uspto-grants-1992_12
特許番号
US05169857

反応ノート

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