반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1Cl.[CH2:10]([NH:12][CH2:13][CH3:14])[CH3:11].O.CC(=O)OCC>C1(C)C=CC=CC=1>[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[N:12]([CH2:13][CH3:14])[CH2:10][CH3:11]참가 물질
6
실험 절차
3,4,6-Trichloropyridazine (2 g) and diethylamine (2.4 ml) were initially charged in toluene (10 ml) and left to stand at RT for 3 days. Then the mixture was admixed with water and EA, and the EA phase was removed. The EA phase was washed three times with water, dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel (70 g cartridge, n-heptane/EA gradient 0-50% within 60 min). 1.1 g of the title compound were obtained.
후처리
- waitleft
- customthe EA phase was removed
- washThe EA phase was washed three times with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified
- customsilica gel (70 g cartridge, n-heptane/EA gradient 0-50% within 60 min)
출처 및 근거
- ORD 기록
- ord-8b427b2e1e5a481394b1b715a71e768f
- 출처 데이터셋
- uspto-grants-2012_06
- 특허 번호
- US08198272B2
연결된 노트
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