Methyl 2-hydroxy-1-naphthoate → Methyl 2-hydroxy-5,6,7,8-tetrahydronaphthalene-1-carboxylate

HRID 631876

반응식

HRID 631876 반응식
[CH3:1][O:2][C:3]([C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][C:6]=1[OH:15])=[O:4].[H][H]>C(O)(=O)C.[Pt]=O>[CH3:1][O:2][C:3]([C:5]1[C:14]2[CH2:13][CH2:12][CH2:11][CH2:10][C:9]=2[CH:8]=[CH:7][C:6]=1[OH:15])=[O:4]

참가 물질

5

반응물 2

HCID 598533Methyl 2-hydroxy-1-naphthoateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 11600901Methyl 2-hydroxy-5,6,7,8-tetrahydronaphthalene-1-carboxylate수율 114.7%

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 176Acetic Acid용매

실험 절차

Under an atmosphere of nitrogen, platinum oxide (5 g) was added to a solution of 2-hydroxy-naphthalene-1-carboxylic acid methyl ester (10 g) in acetic acid (200 mL). The nitrogen atmosphere was replaced by hydrogen, the pressure was increased to 4 bar and the mixture was stirred overnight. The resulting suspension was filtered and the filtrate was concentrated under vacuum to give an oil. The residue was purified by chromatography on silica, eluting with DCM. The fractions containing the desired product were combined and evaporated under vacuum to give the title compound as a colorless oil (11.7 g).

후처리

  1. temperaturethe pressure was increased to 4 bar
  2. filtrationThe resulting suspension was filtered
  3. concentrationthe filtrate was concentrated under vacuum
  4. customto give an oil
  5. customThe residue was purified by chromatography on silica
  6. washeluting with DCM
  7. additionThe fractions containing the desired product
  8. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-eaa2476de1ea47278ce680562c721a0d
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321740B2

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