Ammonia → isobutyl P-(3-aminopropyl)-P-methyl-phosphinate
반응식
[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]참가 물질
6
실험 절차
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).
후처리
- filtrationThe mixture is then filtered
- concentrationthe filtrate is concentrated under reduced pressure
- distillationThe crude product is distilled under reduced pressure
출처 및 근거
- ORD 기록
- ord-346ce8e3169a493f89fa986580fa4503
- 출처 데이터셋
- uspto-grants-1995_10
- 특허 번호
- US05461040
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