Sodium hydride → HCID 54262809, 화합물

HRID 1421718노트

반응식

HRID 1421718 반응식
[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]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 21696991HCID 21696991, 화합물HCID 54057074HCID 54057074, 화합물

생성물 1

HCID 54262809HCID 54262809, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aad64c1a9be64fcc81cd4c12888e7a0a
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06077853

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