Methanol → HCID 67812897, 화합물

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[OH:1][C:2]1[CH:14]=[CH:13][C:5]2[C:6]([CH2:9][C:10]([OH:12])=[O:11])=[CH:7][O:8][C:4]=2[C:3]=1[CH3:15].OS(O)(=O)=O.[CH3:21]O>>[CH3:21][O:11][C:10](=[O:12])[CH2:9][C:6]1[C:5]2[CH:13]=[CH:14][C:2]([OH:1])=[C:3]([CH3:15])[C:4]=2[O:8][CH:7]=1

참가 물질

반응물 3

HCID 887Methanol

HCID 1118Sulfuric Acid

HCID 4738325HCID 4738325, 화합물

생성물 1

HCID 67812897HCID 67812897, 화합물

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온도: 60 °C

실험 절차

To a mixture of (6-hydroxy-7-methyl-1-benzofuran-3-yl)acetic acid (2.61 g) in MeOH (80 mL) was added conc. H2SO4 (0.135 mL). The mixture was stirred at 60° C. for 1 h. The mixture was concentrated. The mixture was neutralized with saturated aqueous NaHCO3 and extracted with EtOAc. The combined organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (2.52 g).

후처리

concentrationThe mixture was concentrated
extractionextracted with EtOAc
washThe combined organic layer was washed with brine
dry with materialdried over MgSO4
concentrationconcentrated in vacuo
customThe residue was purified by silica gel column chromatography (EtOAc/hexane)

출처 및 근거

ORD 기록: ord-dfeed80a6ae941e9a553be9e9ea1a313
출처 데이터셋: uspto-grants-2016_01
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09238639B2

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