Methylamine → HCID 66707598、化合物
反応式
[CH3:1][NH2:2].C[O:4][C:5](=O)[CH2:6][CH2:7][CH:8]1[CH2:13][CH2:12][CH:11]=[CH:10][CH2:9]1>CO>[CH:8]1([CH2:7][CH2:6][C:5]([NH:2][CH3:1])=[O:4])[CH2:13][CH2:12][CH:11]=[CH:10][CH2:9]1参加物
4
実験手順
Methyl amine (8 M in EtOH, 75 ml, 600 mmol) was added to a mixture of 3-cyclohex-3-enyl-propionic acid methyl ester (German patent DE 4023848 A1 19920130) (20.0 g, 119 mmol) in 75 mL of methanol. The mixture was stirred at room temperature for one day. Additional Methyl amine (8 M in EtOH, 40 ml, 320 mmol) was added to the mixture and stirring continued for one more day. The mixture was concentrated and the residue was taken up in ethyl acetate, washed with 0.5 M aqueous HCl, dried and stripped of the solvent to give the title compound (19.50 g, 98% yield, uncorrected) as a pale orange solid.
後処理
- stirringstirring
- concentrationThe mixture was concentrated
- washwashed with 0.5 M aqueous HCl
- customdried
出典と根拠
- ORDレコード
- ord-735a23fd81c94ae09058f180f746e49c
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08153689B2
反応ノート
読み込み中…