Methanol → HCID 178526243, 화합물

HRID 16401

반응식

HRID 16401 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]1

참가 물질

5

반응물 3

HCID 887MethanolHCID 92221H-Pyrrolo(2,3-b)pyridineHCID 70297m-Chloroperbenzoic acid

생성물 1

HCID 178526243HCID 178526243, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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

  1. customwater that separates off is removed
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. temperatureto increase to room temperature
  4. customformed
  5. additionis added
  6. filtrationThe mixture is filtered through silica gel (mobile phase: dichloromethane/methanol 95:5)
  7. customthe product fractions are dried
  8. 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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