Hydrochloric Acid → HCID 178448697, 화합물

HRID 2229402노트

반응식

HRID 2229402 반응식
[CH2:1]([N:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][N:13]=2)[C:8]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH2:22][CH2:23][CH2:24][O:25]CC3C=CC=CC=3)[CH:16]=2)=[C:7]([NH:33][C:34]([NH:36][C:37]2[CH:42]=[C:41]([CH2:43][C:44]3[CH:48]=[CH:47][NH:46][N:45]=3)[CH:40]=[CH:39][C:38]=2[C:49]([CH3:52])([CH3:51])[CH3:50])=[O:35])[C:6]1=[O:53])[CH2:2][CH2:3][CH3:4].Cl>CO.[C].[Pd]>[CH2:1]([N:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][N:13]=2)[C:8]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH2:22][CH2:23][CH2:24][OH:25])[CH:16]=2)=[C:7]([NH:33][C:34]([NH:36][C:37]2[CH:42]=[C:41]([CH2:43][C:44]3[CH:48]=[CH:47][NH:46][N:45]=3)[CH:40]=[CH:39][C:38]=2[C:49]([CH3:52])([CH3:51])[CH3:50])=[O:35])[C:6]1=[O:53])[CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 178448698HCID 178448698, 화합물

생성물 1

HCID 178448697HCID 178448697, 화합물수율 94.6%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

A suspension of N-[1-butyl-4-[3-[3-(benzyloxy)propoxy]phenyl]-1,2-dihydro-2-oxo-1,8-naphthyridin-3-yl]-N′-[2-tert-butyl-5-(1-pyrazolylmethyl)phenyl]urea (1.86 g, 2.6 mmol), 10% palladium carbon (180 mg), conc. hydrochloric acid (0.21 ml, 2.6 mmol) in methanol is stirred under hydrogen atmosphere at room temperature for 8 hours. The mixture is filtered on celite, and the solvent is concentrated under reduced pressure. The resultant is dissolved in chloroform, and thereto are added water and aqueous ammonia. The mixture is stirred and the chloroform layer is dried over anhydrous sodium sulfate, and the solvent is concentrated under reduced pressure. The residue is purified by silica gel column chromatography to give the title compound (1.53 g, 2.46 mmol) as colorless amorphous.

후처리

  1. filtrationThe mixture is filtered on celite
  2. concentrationthe solvent is concentrated under reduced pressure
  3. dissolutionThe resultant is dissolved in chloroform
  4. additionare added water and aqueous ammonia
  5. stirringThe mixture is stirred
  6. dry with materialthe chloroform layer is dried over anhydrous sodium sulfate
  7. concentrationthe solvent is concentrated under reduced pressure
  8. customThe residue is purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-59314a994e3048e18aab489102ba2327
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06420381B1

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