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4-(Bromomethyl)benzene-1,2-dicarbonitrile → HCID 18779782, 화합물

HRID 1421764
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HRID 1421764 반응식
Br[CH2:2][C:3]1[CH:4]=[C:5]([C:11]#[N:12])[C:6](=[CH:9][CH:10]=1)[C:7]#[N:8].[Cl:13][C:14]1[CH:15]=[CH:16][C:17](=[O:51])[N:18]([C:20]2[CH:25]=[CH:24][C:23]([CH2:26][C:27]3[N:28]=[CH:29][N:30](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[CH:31]=3)=[CH:22][N:21]=2)[CH:19]=1>CC#N>[Cl:13][C:14]1[CH:15]=[CH:16][C:17](=[O:51])[N:18]([C:20]2[CH:25]=[CH:24][C:23]([CH2:26][C:27]3[N:28]([CH2:2][C:3]4[CH:4]=[C:5]([C:11]#[N:12])[C:6](=[CH:9][CH:10]=4)[C:7]#[N:8])[CH:29]=[N:30][CH:31]=3)=[CH:22][N:21]=2)[CH:19]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 187797764-(Bromomethyl)benzene-1,2-dicarbonitrileHCID 702869365-chloro-5'-(1-trityl-1H-imidazol-4-ylmethyl)-[1,2']bipyridinyl-2-one

생성물 1

HCID 18779782HCID 18779782, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
60 °C

실험 절차

4-Bromomethyl-phthalonitrile from step 3 (50 mg, 0.28 mmol) and 5-chloro-5'-(1-trityl-1H-imidazol-4-ylmethyl)-[1,2']bipyridinyl-2-one from Example 23, Step 5 (150 mg, 0.28 mmol) were dissolved in CH3CN (1.4 ml) and heated to 60° C. for 16 hours. The solvent was removed in vacuo and redissolved in MeOH (1.4 ml). The reaction mixture was heated to 60° C. for several hours. Solvent was removed in vacuo and the resulting residue was purified by flash chromatography [4% MeOH(5% NH4OH)/CH2Cl2 ] to yield the final product.

후처리

  1. customThe solvent was removed in vacuo
  2. dissolutionredissolved in MeOH (1.4 ml)
  3. temperatureThe reaction mixture was heated to 60° C. for several hours
  4. customSolvent was removed in vacuo
  5. customthe resulting residue was purified by flash chromatography [4% MeOH(5% NH4OH)/CH2Cl2 ]

출처 및 근거

ORD 기록
ord-20218999fa704685ba1724a058dee1ec
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06077853

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