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Sodium hydride → HCID 10690257, 화합물

HRID 1886074
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HRID 1886074 반응식
[H-].[Na+].[CH3:3][C:4]1[N:5]=[C:6]([CH3:15])[C:7]2[C:8](=[N:10][C:11](=[O:14])[CH2:12][CH:13]=2)[N:9]=1.Br[CH2:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]2[CH:31]=[CH:30][CH:29]=[CH:28][C:25]=2[C:26]#[N:27])=[CH:20][CH:19]=1>CN(C=O)C>[CH3:3][C:4]1[N:5]=[C:6]([CH3:15])[C:7]2[CH:13]=[CH:12][C:11](=[O:14])[N:10]([CH2:17][C:18]3[CH:19]=[CH:20][C:21]([C:24]4[CH:31]=[CH:30][CH:29]=[CH:28][C:25]=4[C:26]#[N:27])=[CH:22][CH:23]=3)[C:8]=2[N:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 15019124'-(Bromomethyl)-2-cyanobiphenylHCID 67696840HCID 67696840, 화합물

생성물 1

HCID 10690257HCID 10690257, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

Using the same procedure as described in Step 1 of Example 8, to a stirred suspension of NaH (60% dispersion in mineral oil) in DMF add 2,4-dimethyl-7H-pyrido[2,3-d]pyrimidin-7-one, prepared according to T. Sakamoto, et al. Chem. Pharm. Bull., 1982, 30, 2410. After 45 min, add 2-[4-(bromomethyl)phenyl]benzonitrile in DMF and stir the mixture at room temperature for 18 h. Add water and extract the mixture with CH2Cl2. Concentrate the extracts and purify the crude product by flash chromatography (2% MeOH/CH2Cl2). Trituration with ether gives the product.

후처리

  1. customprepared
  2. extractionAdd water and extract the mixture with CH2Cl2
  3. concentrationConcentrate the extracts
  4. custompurify the crude product by flash chromatography (2% MeOH/CH2Cl2)
  5. customTrituration with ether gives the product

출처 및 근거

ORD 기록
ord-8dc30d9dbc0b43d2a502d6db52c0c6df
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05149699

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