Diethyl Ether → N'-[(3-chlorobenzoyl)oxy]-2-hydroxypropanimidamide
反応式
[OH:1][N:2]=[C:3]([NH2:7])[CH:4]([OH:6])[CH3:5].[Cl:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12](Cl)=[O:13].CCOCC>C1COCC1>[Cl:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12]([O:1][N:2]=[C:3]([NH2:7])[CH:4]([OH:6])[CH3:5])=[O:13]参加物
5
実験手順
6.45 g crude N′,2-dihydroxypropanimidamide was cooled on an ice-bath with 23.5 mL DEA in THF (200 mL). To this slurry 21.94 g 3-chlorobenzoyl chloride was added. The mixture was warmed to r.t. and stirred for 2 h. Addition of Et2O (200 mL), washing with sat. aq. NH4Cl and re-extraction of the aq. layer gave after combining and concentration of the org. layers followed by drying in vacuo 27.24 g of crude title compound, which was directly used in the next step. LC-MS (M++1): 243.
後処理
- washwashing with sat. aq. NH4Cl and re-extraction of the aq. layer
- customgave
- dry with materialby drying in vacuo 27.24 g of crude title compound, which
出典と根拠
- ORDレコード
- ord-7266d1236a3d442db599bed65fa89002
- 出典データセット
- uspto-grants-2009_08
- 特許番号
- US07576077B2
反応ノート
読み込み中…