Methanol → HCID 67812897、化合物

反応式

[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

参加物

反応物 3

HCID 887Methanol

HCID 1118Sulfuric Acid

HCID 4738325HCID 4738325、化合物

生成物 1

HCID 67812897HCID 67812897、化合物

反応条件

温度: 60 °C

実験手順

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).

後処理

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)

出典と根拠

ORDレコード: ord-dfeed80a6ae941e9a553be9e9ea1a313
出典データセット: uspto-grants-2016_01
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09238639B2

反応ノート

読み込み中…

参加物