Water → HCID 54136706、化合物

HRID 1440983ノート

反応式

HRID 1440983 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](OCC)=[O:23])=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[K+]>O1CCCC1>[OH:23][CH2:22][C:9]1[C:10]([CH:19]([CH3:21])[CH3:20])=[N:11][C:12]([CH3:18])=[C:13]([CH2:14][OH:15])[C:8]=1[C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=1

参加物

6

反応物 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 10155368HCID 10155368、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 54136706HCID 54136706、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

20.7 g (57.7 mmol) of the compound from Example 26 dissolved in 50 ml of absolute tetrahydrofuran are slowly added dropwise under nitrogen to a suspension of 6 g (158 mmol) of lithium aluminum hydride in 200 ml of absolute tetrahydrofuran at 60° C. The mixture is heated to reflux for 1 h, cooled to 0° C. and 18 ml of water are cautiously added. 6 ml of 10% strength potassium hydroxide solution are added to the mixture, it is filtered off from the precipitate with suction and the residue is boiled twice using 250 ml of ether each time. The combined mother liquors are dried over magnesium sulphate and concentrated in vacuo, The residue is stirred with petroleum ether, filtered off with suction and dried in a desiccator.

後処理

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 1 h
  3. filtrationis filtered off from the precipitate with suction
  4. dry with materialThe combined mother liquors are dried over magnesium sulphate
  5. concentrationconcentrated in vacuo
  6. filtrationfiltered off with suction
  7. customdried in a desiccator

出典と根拠

ORDレコード
ord-2609530195684d0abe5f91e31b0f6633
出典データセット
uspto-grants-1996_03
特許番号
US05502057

反応ノート

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