Formic Acid → HCID 89996059、化合物

反応式

[CH3:1][O:2][C:3]1[C:8]([NH2:9])=[CH:7][CH:6]=[C:5]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[N:4]=1.[CH:16](O)=[O:17]>>[CH3:1][O:2][C:3]1[C:8]([NH:9][CH:16]=[O:17])=[CH:7][CH:6]=[C:5]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[N:4]=1

参加物

反応物 2

HCID 284Formic Acid

HCID 12152132526184-47-4

生成物 1

HCID 89996059HCID 89996059、化合物収率 88%

実験手順

A solution of 2-methoxy-6-morpholinopyridin-3-amine (Preparation 70, 40 mg, 0.191 mmol) in formic acid (3 mL) was heated to reflux for 3 hours. The reaction mixture was concentrated in vacuo. The residue was partitioned between aqueous saturated NaHCO3 (40 mL) and EtOAc (40 mL). The aqueous layer was re-extracted with EtOAc (40 mL). The combined organic layers were washed with water (40 mL) and brine (40 mL), dried (MgSO4) and concentrated in vacuo, to give the title compound (40 mg, 88%).

後処理

temperatureto reflux for 3 hours
concentrationThe reaction mixture was concentrated in vacuo
customThe residue was partitioned between aqueous saturated NaHCO3 (40 mL) and EtOAc (40 mL)
extractionThe aqueous layer was re-extracted with EtOAc (40 mL)
washThe combined organic layers were washed with water (40 mL) and brine (40 mL)
dry with materialdried (MgSO4)
concentrationconcentrated in vacuo

出典と根拠

ORDレコード: ord-32ce2748e4284442922b4f18630c6df5
出典データセット: uspto-grants-2016_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09409907B2

反応ノート

読み込み中…

参加物