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Sodium Hydroxide → HCID 67339697, 화합물

HRID 1675080
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HRID 1675080 반응식
[F:1][C:2]([F:32])([F:31])[C:3]1[N:7]2[N:8]=[C:9]([N:12]3[CH2:17][CH2:16][CH:15]([C:18]4[C:26]5[C:21](=[CH:22][CH:23]=[C:24]([C:27]([O:29]C)=[O:28])[CH:25]=5)[NH:20][CH:19]=4)[CH2:14][CH2:13]3)[CH:10]=[CH:11][C:6]2=[N:5][N:4]=1.[OH-].[Na+]>CO>[F:32][C:2]([F:1])([F:31])[C:3]1[N:7]2[N:8]=[C:9]([N:12]3[CH2:17][CH2:16][CH:15]([C:18]4[C:26]5[C:21](=[CH:22][CH:23]=[C:24]([C:27]([OH:29])=[O:28])[CH:25]=5)[NH:20][CH:19]=4)[CH2:14][CH2:13]3)[CH:10]=[CH:11][C:6]2=[N:5][N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 67340259HCID 67340259, 화합물

생성물 1

HCID 67339697HCID 67339697, 화합물수율 89.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl 3-[1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]-1H-indole-5-carboxylate (3.28 g, 7.38 mmol) and 2M NaOH (10 mL, 7.38 mmol) in methanol (80 mL) were heated under reflux for 40 hours. The resulting solution was concentrated by evaporation, then acidified to pH 2-3 with 2M hydrochloric acid to give a colourless precipitate. The precipitate was collected by filtration, washed sequentially with water, acetonitrile and ether and dried under vacuum to afford 3-[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]-1H-indole-5-carboxylic acid (2.83 g, 89%) as a colourless solid.

후처리

  1. temperatureunder reflux for 40 hours
  2. concentrationThe resulting solution was concentrated by evaporation
  3. customto give a colourless precipitate
  4. filtrationThe precipitate was collected by filtration
  5. washwashed sequentially with water, acetonitrile and ether
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-16be4d9ad7c24fcd9b3128553ba51960
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08003649B2

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