Sulfuric Acid → HCID 178438224、化合物

反応式

[CH2:1]([C:3]1([CH:8]([F:13])[C:9]([NH:11][OH:12])=[O:10])OCCO1)[CH3:2].OS(O)(=O)=O>>[CH2:1]([C:3]1[O:12][N:11]=[C:9]([OH:10])[C:8]=1[F:13])[CH3:2]

参加物

反応物 2

HCID 1118Sulfuric Acid

HCID 866370552-(2-Ethyl-[1,3]dioxolan-2-yl)-2-fluoro-N-hydroxyacetamide

生成物 1

HCID 178438224HCID 178438224、化合物収率 82.1%

実験手順

A sol. of 2-(2-ethyl-[1,3]dioxolan-2-yl)-2-fluoro-N-hydroxyacetamide (502 mg, 2.60 mmol) in cone. H2SO4 (1.2 mL) was stirred for 2 h at rt, then for 2 h at 50° C. The mixture was poured onto ice, and this mixture was extracted with EtOAc. The combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Drying the residue under high vacuum yielded the title compound (280 mg, 82%). LC-MS: tR=0.66, ES+: not visible.

後処理

additionThe mixture was poured onto ice
extractionthis mixture was extracted with EtOAc
dry with materialextracts were dried over MgSO4
filtrationfiltered
customthe solvents were removed under reduced pressure
customDrying the residue under high vacuum

出典と根拠

ORDレコード: ord-34d778ebad034d348b7d33d7373bd868
出典データセット: uspto-grants-2012_03
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08138340B2

反応ノート

読み込み中…

参加物