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Potassium Carbonate → HCID 86695573, 화합물

HRID 1465689
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HRID 1465689 반응식
Cl.N1(S([N:10]=[N+:11]=[N-])(=O)=O)C=CN=C1.[NH2:13][C@@H:14]1[CH2:19][CH2:18][CH2:17][N:16]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:15]1.C([O-])([O-])=O.[K+].[K+]>CO>[N:13]([C@@H:14]1[CH2:19][CH2:18][CH2:17][N:16]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:15]1)=[N+:10]=[N-:11]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1501974tert-butyl (3R)-3-aminopiperidine-1-carboxylateHCID 235839821H-imidazole-1-sulfonyl azide hydrochloride

생성물 1

HCID 86695573HCID 86695573, 화합물수율 57.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Imidazole-1-sulfonyl azide hydrochloride (1.03 g, 6.0 mmol) was added to (R)-tert-butyl 3-aminopiperidine-1-carboxylate (1.0 g, 5.0 mmol), K2CO3 (1.33 g, 10.0 mmol) and CuSO4.5H2O (0.012 g, 0.05 mmol) in MeOH (30 mL) and the mixture was stirred at room temperature for 12 h. The mixture was concentrated, diluted with H2O (50 mL), extracted with EtOAc (3×60 mL). The combined organic layers were dried (MgSO4), filtered and concentrated to give (R)-tert-butyl 3-azidopiperidine-1-carboxylate (0.65 g).

후처리

  1. concentrationThe mixture was concentrated
  2. additiondiluted with H2O (50 mL)
  3. extractionextracted with EtOAc (3×60 mL)
  4. dry with materialThe combined organic layers were dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c8283b2774f74b2aafbfe60944c148b8
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08999966B2

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