Triethylamine → HCID 67220707, 화합물

HRID 1865025노트

반응식

HRID 1865025 반응식
C(N(CC)CC)C.Cl.Cl[C:10]1[N:18]=[CH:17][CH:16]=[CH:15][C:11]=1[C:12]([OH:14])=O.[CH:19]1([CH2:22][NH:23][C:24]2[C:25]([S:43][CH3:44])=[N:26][N:27]3[C:32]([C:33]4[C:38]([CH3:39])=[CH:37][C:36]([CH3:40])=[CH:35][C:34]=4[O:41][CH3:42])=[CH:31][CH:30]=[CH:29][C:28]=23)[CH2:21][CH2:20]1.C(=O)([O-])O.[Na+]>ClCCl.C(OCC)(=O)C>[CH:19]1([CH2:22][N:23]([C:24]2[C:25]([S:43][CH3:44])=[N:26][N:27]3[C:32]([C:33]4[C:38]([CH3:39])=[CH:37][C:36]([CH3:40])=[CH:35][C:34]=4[O:41][CH3:42])=[CH:31][CH:30]=[CH:29][C:28]=23)[C:12](=[O:14])[C:11]2[CH:15]=[CH:16][CH:17]=[N:18][CH:10]=2)[CH2:20][CH2:21]1

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 27628002-Chloronicotinic acid hydrochlorideHCID 21984576N-cyclopropylmethyl-N-[7-(2-methoxy-4,6-dimethylphenyl)-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]amine

생성물 1

HCID 67220707HCID 67220707, 화합물수율 84.8%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

Triethylamine (0.038 mL) and chloronicotinic acid hydrochloride (20 mg) were added to a solution of N-cyclopropylmethyl-N-[7-(2-methoxy-4,6-dimethylphenyl)-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]amine (33 mg) in dichloromethane (0.8 mL) while cooling on ice, and the mixture was stirred at the same temperature for 1 hour. Saturated aqueous sodium hydrogencarbonate was added while cooling on ice, extraction was performed with ethyl acetate, and the extract washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=3:2) to obtain the title compound (36 mg) as white crystals.

후처리

  1. temperaturewhile cooling on ice
  2. temperaturewhile cooling on ice, extraction
  3. washthe extract washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=3:2)

출처 및 근거

ORD 기록
ord-2d86c59e6ba446a6a355f3cb5387bb55
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625925B2

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