Methylamine → 4-[1,3]Dioxan-2-yl-N-methyl-butyramide
反応式
[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[CH2:7][CH2:8][CH2:9][C:10]([OH:12])=O.CN.Cl.[CH3:16][N:17](C)CCCN=C=NCC.OC1C2N=NNC=2C=CC=1>ClCCl>[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[CH2:7][CH2:8][CH2:9][C:10]([NH:17][CH3:16])=[O:12]参加物
6
実験手順
To 4-[1,3]dioxan-2-yl-butyric acid (2.55 g, 0.015 mol) in dichloromethane (200 ml) was added methylamine (2M in THF, 8.1 ml, 0.016 mol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (3.09 g, 0.016 mol) and hydroxybenzotriazole (2.16 g, 0.016 mol) and the mixture stirred at room temperature overnight. The organic layer was washed with saturated sodium bicarbonate solution (200 ml) and the aqueous layer extracted with dichloromethane (4×50 ml). The combined organics were dried (Na2SO4) and evaporated to give a colourless oil (3.2 g)
後処理
- washThe organic layer was washed with saturated sodium bicarbonate solution (200 ml)
- extractionthe aqueous layer extracted with dichloromethane (4×50 ml)
- dry with materialThe combined organics were dried (Na2SO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-45ea3b8591ff4b7bb3fddd7fcac0af8f
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07429579B2
反応ノート
読み込み中…