Dibutyl 4-benzyloxybenzylphosphonate → Dibutyl 4-hydroxybenzylphosphonate

HRID 1488342노트

반응식

HRID 1488342 반응식
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

참가 물질

5

반응물 2

HCID 22904634Dibutyl 4-benzyloxybenzylphosphonateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 22904633Dibutyl 4-hydroxybenzylphosphonate

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c05ff1b3ffd0424c800bd42612b21eba
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05674482

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