Dibutyl 4-benzyloxybenzylphosphonate → Dibutyl 4-hydroxybenzylphosphonate

HRID 1488342ノート

反応式

HRID 1488342 の反応式
C([O:8][C:9]1[CH:27]=[CH:26][C:12]([CH2:13][P:14](=[O:25])([O:20][CH2:21][CH2:22][CH2:23][CH3:24])[O:15][CH2:16][CH2:17][CH2:18][CH3:19])=[CH:11][CH:10]=1)C1C=CC=CC=1.[H][H]>C(OCC)(=O)C.[Pd]>[OH:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:13][P:14](=[O:25])([O:15][CH2:16][CH2:17][CH2:18][CH3:19])[O:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:26][CH:27]=1

参加物

5

反応物 2

HCID 22904634Dibutyl 4-benzyloxybenzylphosphonateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 22904633Dibutyl 4-hydroxybenzylphosphonate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of dibutyl 4-benzyloxybenzylphosphonate (4.07 g) in ethyl acetate (60 ml) is added 10% palladium on carbon (0.41 g) and the mixture shaken under 25 psi of hydrogen for about 20 hours. The mixture is filtered, concentrated in vacuo, and the residue purified by HPLC, eluting with a gradient of 50-65% ethyl acetate in hexane, to give dibutyl 4-hydroxybenzylphosphonate.

後処理

  1. filtrationThe mixture is filtered
  2. concentrationconcentrated in vacuo
  3. customthe residue purified by HPLC
  4. washeluting with a gradient of 50-65% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-c05ff1b3ffd0424c800bd42612b21eba
出典データセット
uspto-grants-1997_10
特許番号
US05674482

反応ノート

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