(R)-1-Boc-piperidine-3-carboxylic acid hydrazide → HCID 178451955, 화합물

HRID 1465698노트

반응식

HRID 1465698 반응식
Cl.[Br:2][C:3]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12](=[NH:16])OCC)[CH:10]=2)[NH:5][N:4]=1.[NH:17]([C:19]([C@@H:21]1[CH2:26][CH2:25][CH2:24][N:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:22]1)=O)[NH2:18]>CO>[Br:2][C:3]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12]3[N:16]=[C:19]([C@@H:21]4[CH2:26][CH2:25][CH2:24][N:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:22]4)[NH:17][N:18]=3)[CH:10]=2)[NH:5][N:4]=1

참가 물질

4

반응물 2

HCID 29922274(R)-1-Boc-piperidine-3-carboxylic acid hydrazideHCID 178468222HCID 178468222, 화합물

생성물 1

HCID 178451955HCID 178451955, 화합물수율 99.4%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
85 °C

실험 절차

Mixture of ethyl 3-bromo-1H-indazole-5-carbimidate hydrochloride (4.1 g, 13.5 mmol) and (R)-tert-butyl 3-(hydrazinecarbonyl)piperidine-1-carboxylate (5.1 g, 20 mmol) in MeOH (25 ml) was heated in a sealed tube at 85° C. overnight. After solvent was evaporated, the residue was diluted with DCM (200 ml) and washed with H2O (50 ml), Dried over Na2SO4; filtered and evaporated solvent. Chromatographed residue eluting with 5% MeOH/DCM to yield (R)-tert-butyl 3-(3-(3-bromo-1H-indazol-5-yl)-1H-1,2,4-triazol-5-yl)piperidine-1-carboxylate as a white solid (6 g).

후처리

  1. customAfter solvent was evaporated
  2. additionthe residue was diluted with DCM (200 ml)
  3. washwashed with H2O (50 ml)
  4. dry with materialDried over Na2SO4
  5. filtrationfiltered
  6. customevaporated solvent
  7. washChromatographed residue eluting with 5% MeOH/DCM

출처 및 근거

ORD 기록
ord-f00ab3c41a09404ba85886140ca3c237
출처 데이터셋
uspto-grants-2015_04
특허 번호
US08999966B2

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