Methanol → HCID 178526243, 화합물
반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[NH:12]1[C:16]2=[N:17][CH:18]=[CH:19][CH:20]=[C:15]2[CH:14]=[CH:13]1.CO>ClCCl>[NH:12]1[C:16]2=[N+:17]([O-:9])[CH:18]=[CH:19][CH:20]=[C:15]2[CH:14]=[CH:13]1참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
539.7 g (2.35 mol) of 3-chloroperbenzoic acid are dissolved in 6.11 l of dichloromethane, and water that separates off is removed. The organic phase is dried over sodium sulfate and cooled to 0° C. A solution of 163 g (1.38 mol) of 1H-pyrrolo[2,3-b]pyridine in 1.00 l of dichloromethane is then added, and the temperature is allowed to increase to room temperature. After 2 hours, sufficient methanol to re-dissolve the precipitate formed is added. The mixture is filtered through silica gel (mobile phase: dichloromethane/methanol 95:5) and the product fractions are dried after concentration under high vacuum.
후처리
- customwater that separates off is removed
- dry with materialThe organic phase is dried over sodium sulfate
- temperatureto increase to room temperature
- customformed
- additionis added
- filtrationThe mixture is filtered through silica gel (mobile phase: dichloromethane/methanol 95:5)
- customthe product fractions are dried
- concentrationafter concentration under high vacuum
출처 및 근거
- ORD 기록
- ord-9895e424d20e49a3b999223b13d4f924
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07737153B2
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