반응식
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[K+]>O1CCCC1>[CH2:1]([N:8]1[CH2:4][CH2:3][CH:2]([NH:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:1]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1참가 물질
실험 절차
1,000 g (5.34 mols) of 1-benzyl-Δ3 -pyrroline-2,5-dione are dissolved in 2.5 l of tetrahydrofuran, and 572 g (5.34 mols) of benzylamine are added with stirring at 10° to 20° C. The mixture is left to stand for 24 hours at room temperature, after which 360 g are removed from the resulting solution (3,848 g of total weight) and added to a solution of 38 g (1 mol) of lithium aluminum hydride in 380 ml of absolute dehydrated tetrahydrofuran. The mixture is refluxed for 20 hours, 500 ml of tetrahydrofuran, 38 g of water and 120 ml of tetrahydrofuran, 38 g of 10% strength potassium hydroxide solution and 114 g of water are then sucessively added to the mixture. The salts are filtered off with suction, washed with tetrahydrofuran, the filtrate is concentrated, and the residue is distilled.
후처리
- waitThe mixture is left
- customafter which 360 g are removed from the resulting solution (3,848 g of total weight)
- temperatureThe mixture is refluxed for 20 hours
- filtrationThe salts are filtered off with suction
- washwashed with tetrahydrofuran
- concentrationthe filtrate is concentrated
- distillationthe residue is distilled
출처 및 근거
- ORD 기록
- ord-88a4f23619b44c5baad87a92b773ac16
- 출처 데이터셋
- uspto-grants-1990_03
- 특허 번호
- US04910319
연결된 노트
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