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Pyrrolidine → HCID 67313348、化合物

HRID 1010885
ノート
印刷プレビュー

反応式

HRID 1010885 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C@@H:11]([NH:13][C:14]2[N:19]=[C:18]([C:20]3[N:24]4[CH:25]=[CH:26][CH:27]=[C:28]([CH3:29])[C:23]4=[N:22][CH:21]=3)[C:17]([C:30]#[N:31])=[CH:16][N:15]=2)[CH3:12])=[CH:7][CH:6]=1)=[O:4].[NH:32]1[CH2:36][CH2:35][CH2:34][CH2:33]1.C(=O)([O-])O.[Na+]>CN(C)C=O>[CH3:29][C:28]1[C:23]2[N:24]([C:20]([C:18]3[C:17]([C:30]#[N:31])=[CH:16][N:15]=[C:14]([NH:13][C@H:11]([C:8]4[CH:9]=[CH:10][C:5]([C:3](=[O:4])[CH2:2][N:32]5[CH2:36][CH2:35][CH2:34][CH2:33]5)=[CH:6][CH:7]=4)[CH3:12])[N:19]=3)=[CH:21][N:22]=2)[CH:25]=[CH:26][CH:27]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 31268PyrrolidineHCID 516892Sodium BicarbonateHCID 86625211HCID 86625211、化合物

生成物 1

HCID 67313348HCID 67313348、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

20 mg of the compound [3-2] was dissolved in 0.4 mL of N,N-dimethylformamide, and 7 μL of pyrrolidine was added thereto. The reaction mixture was stirred for 30 minutes at room temperature, and then thereto was added a saturated aqueous solution of sodium hydrogen carbonate, and the mixture was extracted with chloroform. The resulting organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The insolubles were filtered, the filtrate was concentrated under reduced pressure, and the resulting residue was purified by preparative thin-layer chromatography, to obtain 3 mg of 4-(8-methylimidazo[1,2-a]pyridin-3-yl)-2-({(1S)-1-[4-(pyrrolidin-1-ylacetyl) phenyl]ethyl}amino)pyrimidine-5-carbonitrile [3-3] (hereinafter, referred to as the compound [3-3]) as a colorless oily product.

後処理

  1. extractionthe mixture was extracted with chloroform
  2. washThe resulting organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationThe insolubles were filtered
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customthe resulting residue was purified by preparative thin-layer chromatography

出典と根拠

ORDレコード
ord-60cd8e9b9b9e48e79df988c1fe8f40dd
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977336B2

反応ノート

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