Hydrochloric Acid → HCID 178448697、化合物

HRID 2229402ノート

反応式

HRID 2229402 の反応式
[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]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 178448698HCID 178448698、化合物

生成物 1

HCID 178448697HCID 178448697、化合物収率 94.6%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-59314a994e3048e18aab489102ba2327
出典データセット
uspto-grants-2002_07
特許番号
US06420381B1

反応ノート

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