(R)-1-Boc-piperidine-3-carboxylic acid hydrazide → HCID 178451955、化合物

HRID 1465698ノート

反応式

HRID 1465698 の反応式
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

参加物

4

反応物 2

HCID 29922274(R)-1-Boc-piperidine-3-carboxylic acid hydrazideHCID 178468222HCID 178468222、化合物

生成物 1

HCID 178451955HCID 178451955、化合物収率 99.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
85 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f00ab3c41a09404ba85886140ca3c237
出典データセット
uspto-grants-2015_04
特許番号
US08999966B2

反応ノート

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