Methanol → HCID 68705008、化合物

反応式

O=S(Cl)Cl.[S:5]1[C:9]2[CH:10]=[C:11]([CH2:14][C:15]([OH:17])=[O:16])[CH:12]=[CH:13][C:8]=2[N:7]=[CH:6]1.[CH3:18]O>>[CH3:18][O:16][C:15](=[O:17])[CH2:14][C:11]1[CH:12]=[CH:13][C:8]2[N:7]=[CH:6][S:5][C:9]=2[CH:10]=1

参加物

反応物 3

HCID 887Methanol

HCID 24386Thionyl Chloride

HCID 22038417(1,3-Benzothiazol-6-yl)acetic acid

生成物 1

HCID 68705008HCID 68705008、化合物

実験手順

SOCl2 (13.5 g, 114.0 mmol) was added dropwise to a stirred solution of benzothiazol-6-yl-acetic acid (20.0 g, 103.6 mmol) in 150 ml of methanol at 0° C. under N2. After stirring for 2 hours at room temperature the solvent was evaporated and the residue was diluted with ethyl acetate (150 ml). The mixture was washed with saturated sodium carbonate solution (100 ml×3) and brine (100 ml) and then concentrated in vacuo. The residue was purified by column chromatoghaphy eluting with ethyl acetate/petroleum ether (1:5) to return the title compound as a pale yellow oil (15.0 g, 71.5%).

後処理

customwas evaporated
additionthe residue was diluted with ethyl acetate (150 ml)
washThe mixture was washed with saturated sodium carbonate solution (100 ml×3) and brine (100 ml)
concentrationconcentrated in vacuo
customThe residue was purified by column chromatoghaphy
washeluting with ethyl acetate/petroleum ether (1:5)

出典と根拠

ORDレコード: ord-4412a922899a405aa9a99ae8d3e95fc0
出典データセット: uspto-grants-2011_12
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08071581B2

反応ノート

読み込み中…

参加物