Sodium hydride → HCID 54262809、化合物

HRID 1421718ノート

反応式

HRID 1421718 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]2[NH:14][CH:15]=[N:16][C:10]=2[CH:9]1[C:17]1[CH:22]=[CH:21][C:20]([C:23]#[N:24])=[CH:19][CH:18]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Br[CH2:26][C:27]1[CH:28]=[CH:29][C:30]([N:33]2[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:34]2=[O:40])=[N:31][CH:32]=1.[H-].[Na+]>CN(C=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]2[N:14]=[CH:15][N:16]([CH2:26][C:27]3[CH:28]=[CH:29][C:30]([N:33]4[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:34]4=[O:40])=[N:31][CH:32]=3)[C:10]=2[CH:9]1[C:17]1[CH:18]=[CH:19][C:20]([C:23]#[N:24])=[CH:21][CH:22]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 21696991HCID 21696991、化合物HCID 54057074HCID 54057074、化合物

生成物 1

HCID 54262809HCID 54262809、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4-(4-Cyano-phenyl)-1,4,6,7-tetrahydro-imidazo[4,5-c]pyridine-5-carboxylic acid tert-butyl ester (0.16 g, 0.50 mmol) and 5'-bromomethyl-5-chloro-[1,2']bipyridinyl-2-one (Example 10, Step 2)(0.15 g, 0.50 mmol) were dissolved in DMF (6 mL). NaH (0.02 g, 0.60 mmol) was added and stirred at RT under Ar for 1.5 h. The reaction was concentrated in vacuo and partitioned between EtOAc and satd NaHCO3 soln, washed with H2O, brine, dried (MgSO4), filtered and concentrated to give the title compound as a mixture of racemic regloisomers.

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. custompartitioned between EtOAc
  3. washwashed with H2O, brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-aad64c1a9be64fcc81cd4c12888e7a0a
出典データセット
uspto-grants-2000_06
特許番号
US06077853

反応ノート

読み込み中…