Triethylamine → HCID 67220707、化合物

HRID 1865025ノート

反応式

HRID 1865025 の反応式
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

参加物

7

反応物 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

生成物 1

HCID 67220707HCID 67220707、化合物収率 84.8%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2d86c59e6ba446a6a355f3cb5387bb55
出典データセット
uspto-grants-2009_12
特許番号
US07625925B2

反応ノート

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