반응식
[CH:1]([N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1)([CH3:3])[CH3:2].C1COCC1.[OH-].[Na+].[CH:17]([C:19]1[CH:27]=[CH:26][C:22]([C:23](Cl)=[O:24])=[CH:21][CH:20]=1)=[O:18]>O>[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:17]([C:19]2[CH:27]=[CH:26][C:22]([CH:23]=[O:24])=[CH:21][CH:20]=2)=[O:18])[CH2:6][CH2:5]1)([CH3:3])[CH3:2]참가 물질
반응 조건
- 온도
- 2.5 °C
실험 절차
4-Isopropyl-piperazine (79.53 g, 0.620 mol), THF (444 g, 5.04 mol), water (36 g, 2 mol) and a 50% solution of sodium hydroxide (130.6 g, 1.63 mol) were charged to a reaction vessel and cooled to 0-5° C. 4-Formyl-benzoyl chloride in THF (110.08 g, 0.630 mol) was added to the 4-isopropyl-piperazine reaction mixture while maintaining the temperature below about 10° C. The resulting white suspension was stirred at room temperature until the reaction was deemed complete. Water was added to the reaction slurry and the resulting hazy solution was filtered over Celite to remove insolubles. The filtered reaction solution was settled and the water layer was removed. The product/THF layer was dried sequentially with magnesium sulfate and molecular sieves. The product solution (KF≦0.5%) was stored at 5° C. for use without further manipulations.
후처리
- temperaturewhile maintaining the temperature below about 10° C
- filtrationthe resulting hazy solution was filtered over Celite
- customto remove insolubles
- customThe filtered reaction solution
- customthe water layer was removed
- dry with materialThe product/THF layer was dried sequentially with magnesium sulfate and molecular sieves
- customwas stored at 5° C. for use without further manipulations
출처 및 근거
- ORD 기록
- ord-aec267aab7a3492ea2e6faaccc86e556
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07728129B2
연결된 노트
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