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Water → HCID 58970690, 화합물

HRID 598044
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HRID 598044 반응식
[NH2:1][C:2]1[C:11]2[N:12]=[C:13]([CH2:24][O:25][CH2:26][CH3:27])[N:14]([CH2:15][C:16]([NH:19][S:20]([CH3:23])(=[O:22])=[O:21])([CH3:18])[CH3:17])[C:10]=2[C:9]2[N:8]=[CH:7][C:6](Br)=[CH:5][C:4]=2[N:3]=1.[OH:29][CH2:30][C:31]1[CH:32]=[C:33](B(O)O)[CH:34]=[CH:35][CH:36]=1.C(=O)([O-])[O-].[Na+].[Na+].O>C(O)CC.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[NH2:1][C:2]1[C:11]2[N:12]=[C:13]([CH2:24][O:25][CH2:26][CH3:27])[N:14]([CH2:15][C:16]([NH:19][S:20]([CH3:23])(=[O:22])=[O:21])([CH3:18])[CH3:17])[C:10]=2[C:9]2[N:8]=[CH:7][C:6]([C:35]3[CH:34]=[CH:33][CH:32]=[C:31]([CH2:30][OH:29])[CH:36]=3)=[CH:5][C:4]=2[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 2734662[3-(Hydroxymethyl)phenyl]boronic acidHCID 58970687HCID 58970687, 화합물

생성물 1

HCID 58970690HCID 58970690, 화합물수율 77.1%

시약·촉매·용매 3

HCID 11776Triphenylphosphine
촉매
HCID 167845palladium(II) acetate촉매
HCID 10311-Propanol용매

실험 절차

The method described in Example 152 was used to treat N-{2-[4-amino-7-bromo-2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-1,1-dimethylethyl}methanesulfonamide (1.2 g, 2.55 mmol) and 3-(hydroxymethyl)benzeneboronic acid (0.58 g, 3.8 mmol) in 1-propanol (15 mL) with triphenylphosphine (20.0 mg, 0.0760 mmol), aqueous sodium carbonate (3.82 mL of 2 M), water (3 mL), and palladium (II) acetate (5.7 mg, 0.025 mmol) with the following modifications. The reaction mixture was heated at reflux overnight. The crude product was purified by automated flash chromatography (FLASH 40+M cartridge, eluting with 0% to 35% CMA in chloroform) followed by recrystallization from acetonitrile to provide 0.98 g of N-(2-{4-amino-2-(ethoxymethyl)-7-[3-(hydroxymethyl)phenyl]-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl}-1,1-dimethylethyl)methanesulfonamide as a white solid, mp 173-174° C.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux overnight
  3. customThe crude product was purified by automated flash chromatography (FLASH 40+M cartridge, eluting with 0% to 35% CMA in chloroform)
  4. customfollowed by recrystallization from acetonitrile

출처 및 근거

ORD 기록
ord-816252369d1748a4867ff9475b561a58
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07897609B2

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