반응식
[Cl:1][C:2]1[C:3]([Cl:11])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].Cl[Si](C)(C)C.[CH3:17][CH2:18]O>>[Cl:1][C:2]1[C:3]([Cl:11])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([O:9][CH2:17][CH3:18])=[O:8]참가 물질
4
실험 절차
To a solution of 5,6-dichloronicotinic acid (20.01 g, 104 mmol) in EtOH (500 mL) at 20° C. was added chlorotrimethylsilane (132 mL, 1042 mmol). The reaction was stirred for 72 hours. The reaction mixture was then concentrated and diluted with EtOAc (500 mL), and washed with saturated NaHCO3 (2×100 mL) and brine (100 mL). The organic was then dried (Na2SO4) and concentrated under reduced pressure to give final crude product (21.25 g). LCMS m/z 220.1 (M+H)+, Rt 0.94 min.
후처리
- concentrationThe reaction mixture was then concentrated
- additiondiluted with EtOAc (500 mL)
- washwashed with saturated NaHCO3 (2×100 mL) and brine (100 mL)
- dry with materialThe organic was then dried (Na2SO4)
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-5a45f9597fb941b9ae778f44080a3dfb
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09434719B2
연결된 노트
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