Methanol → HCID 178526243、化合物

HRID 16401

反応式

HRID 16401 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 178526243HCID 178526243、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9895e424d20e49a3b999223b13d4f924
出典データセット
uspto-grants-2010_06
特許番号
US07737153B2

関連ノート

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