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Ethanol → HCID 178521014、化合物

HRID 931271
ノート
印刷プレビュー

反応式

HRID 931271 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6]N=[C:4]([N:11]2[CH2:16][CH2:15][CH2:14][C@@H:13]([C:17]([N:19]3[CH2:23][CH2:22][CH2:21][CH2:20]3)=[O:18])[CH2:12]2)[N:3]=1.[Br:24][C:25]1[CH:26]=[N:27][CH:28]=[C:29]([CH:32]=1)[CH:30]=O.S(S([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].[CH2:43](O)C>O>[Br:24][C:25]1[CH:32]=[C:29]([C:30]2[NH:1][C:2]3=[N:3][C:4]([N:11]4[CH2:16][CH2:15][CH2:14][C@@H:13]([C:17]([N:19]5[CH2:20][CH2:21][CH2:22][CH2:23]5)=[O:18])[CH2:12]4)=[CH:43][CH:6]=[C:7]3[N:8]=2)[CH:28]=[N:27][CH:26]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 702EthanolHCID 146045Sodium dithionateHCID 27847345-Bromo-3-pyridinecarboxaldehydeHCID 89854015Methanone, [(3R)-1-(4-amino-5-nitro-2-pyrimidinyl)-3-piperidinyl]-1-pyrrolidinyl-

生成物 1

HCID 178521014HCID 178521014、化合物収率 60%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
120 °C

実験手順

To a solution of (R)-(1-(4-amino-5-nitropyrimidin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone (0.5 g, 1.5 mmol) in a mixture of ethanol and water were added 5-bromonicotinaldehyde (0.35 g, 1.6 mmol) and sodium dithionate (1.1 g, 5.9 mmol). The reaction mixture was heated to 120° C. for 16 h. The reaction mixture was concentrated and partitioned between water and ethyl acetate. The organics were concentrated under reduced pressure and the resulting crude was purified via preparative TLC to afford (R)-(1-(2-(5-bromopyridin-3-yl)-3H-imidazo[4,5-b]pyridin-5-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone (400 mg, 60%).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. custompartitioned between water and ethyl acetate
  3. concentrationThe organics were concentrated under reduced pressure
  4. customthe resulting crude was purified via preparative TLC

出典と根拠

ORDレコード
ord-e8fd26ce69f34352b461988a968b53c9
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296745B2

反応ノート

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