Water → HCID 23044250、化合物

HRID 1248362ノート

反応式

HRID 1248362 の反応式
C[O:2][C:3]([C:5]1[C:8]2[CH:9]=[C:10]([O:13][CH3:14])[CH:11]=[CH:12][C:7]=2[CH:6]=1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.S(=O)(=O)(O)O>CCOCC>[CH3:14][O:13][C:10]1[CH:11]=[CH:12][C:7]2[CH:6]=[C:5]([CH2:3][OH:2])[C:8]=2[CH:9]=1

参加物

6

反応物 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 21226445Aluminium lithium hydride2 回HCID 541184135-Methoxybenzocyclobutene-1-carboxylic acid methyl ester

生成物 1

HCID 23044250HCID 23044250、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

Over a period of 30 minutes, while stirring, a solution of 1.92 g of 5-methoxybenzocyclobutene-1-carboxylic acid methyl ester in 30 ml of ether is added dropwise to a suspension of 0.21 g of lithium aluminium hydride in 30 ml of ether. The whole is stirred for 1 hour, a further 1.0 g of lithium aluminium hydride is added and stirring is carried out for a further 2 hours. 5 ml of water and, after a short time, 12.5 ml of 2N sulphuric acid are added dropwise thereto, stirring is carried out for 30 minutes and the ether phase is separated off, shaken twice with ether, dried over magnesium sulphate and concentrated to dryness by evaporation. 5-methoxybenzocyclobutene-1-methanol is obtained in the form of a colourless oil.

後処理

  1. stirringThe whole is stirred for 1 hour
  2. stirringstirring
  3. waitis carried out for a further 2 hours
  4. stirringstirring
  5. waitis carried out for 30 minutes
  6. customthe ether phase is separated off
  7. stirringshaken twice with ether
  8. dry with materialdried over magnesium sulphate
  9. concentrationconcentrated to dryness by evaporation

出典と根拠

ORDレコード
ord-b5b3a7087f2c412ba4adfabb345bcc20
出典データセット
uspto-grants-1985_06
特許番号
US04523030

反応ノート

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