HCID 67426414, 화합물 → 1231930-19-0

HRID 2264355노트

반응식

HRID 2264355 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:16]=[N:17][C:18]([N+:21]([O-])=O)=[CH:19][CH:20]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>[Pd].O1CCCC1>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:16]=[N:17][C:18]([NH2:21])=[CH:19][CH:20]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 1

HCID 67426414HCID 67426414, 화합물

생성물 1

HCID 674264061231930-19-0수율 97.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

Add palladium over carbon 10% (0.6 g) to a suspension of 4-(6-nitro-pyridin-3-yloxy)-piperidine-1-carboxylic acid tert-butyl ester (5.65 g) in a mixture tetrahydrofuran (THF)/methanol (30/30 mL/mL). Hydrogenate in a Parr apparatus at 2 atm overnight. Filter through a celite pad, wash with DCM and methanol. Purify by silica gel column chromatography eluting with DCM/methanol (10%)/ammonia (1%) to afford 5 g of the title compound. MS (ES+): m/z=294 (M+H)+.

후처리

  1. customat 2 atm overnight
  2. filtrationFilter through a celite pad
  3. washwash with DCM and methanol
  4. customPurify by silica gel column chromatography
  5. washeluting with DCM/methanol (10%)/ammonia (1%)

출처 및 근거

ORD 기록
ord-0a97c40c1a134722b51d17921741bb7c
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07855211B2

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