Ammonia → isobutyl P-(3-aminopropyl)-P-methyl-phosphinate
反応式
[C:1]([CH2:3][CH2:4][P:5]([CH3:12])(=[O:11])[O:6][CH2:7][CH:8]([CH3:10])[CH3:9])#[N:2].N.[H][H]>C(O)C.[Ni]>[NH2:2][CH2:1][CH2:3][CH2:4][P:5]([CH3:12])(=[O:11])[O:6][CH2:7][CH:8]([CH3:10])[CH3:9]参加物
6
実験手順
A solution of 20.0 g of isobutyl P-(2-cyanoethyl)-P-methyl-phosphinate in 200 ml of ethanol is added to 230.0 g of an 8% solution of ammonia in ethanol. To this are added 15 ml of Raney nickel slurry and the resulting mixture is hydrogenated at 1 bar until hydrogen uptake ceases. The mixture is then filtered and the filtrate is concentrated under reduced pressure. The crude product is distilled under reduced pressure to give isobutyl P-(3-aminopropyl)-P-methyl-phosphinate, b.p. 130°/0.01 mbar, 31P-NMR spectrum: δ=+57.6 ppm (CDCl3).
後処理
- filtrationThe mixture is then filtered
- concentrationthe filtrate is concentrated under reduced pressure
- distillationThe crude product is distilled under reduced pressure
出典と根拠
- ORDレコード
- ord-413614f3d8f5405eb042f681c417c44e
- 出典データセット
- uspto-grants-1994_01
- 特許番号
- US05281747
反応ノート
読み込み中…