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N-bromobutanimide → 3-[5-bromo-2-methyl-4-(6-methyl-pyridin-2-ylmethoxy)-6-oxo-6H-pyrimidin-1-yl]-4-methyl-benzoic acid methyl ester

HRID 2172621
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HRID 2172621 반응식
[CH3:1][O:2][C:3](=[O:28])[C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[C:6]([N:11]2[C:16](=[O:17])[CH:15]=[C:14]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[N:21]=3)[N:13]=[C:12]2[CH3:27])[CH:5]=1.[Br:29]N1C(=O)CCC1=O>ClCCl>[CH3:1][O:2][C:3](=[O:28])[C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[C:6]([N:11]2[C:16](=[O:17])[C:15]([Br:29])=[C:14]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[N:21]=3)[N:13]=[C:12]2[CH3:27])[CH:5]=1
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참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 866862974-methyl-3-[2-methyl-4-(6-methyl-pyridin-2-ylmethoxy)-6-oxo-6H-pyrimidin-1-yl]-benzoic acid methyl ester

생성물 1

HCID 866862983-[5-bromo-2-methyl-4-(6-methyl-pyridin-2-ylmethoxy)-6-oxo-6H-pyrimidin-1-yl]-4-methyl-benzoic acid methyl ester수율 100.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-methyl-3-[2-methyl-4-(6-methyl-pyridin-2-ylmethoxy)-6-oxo-6H-pyrimidin-1-yl]-benzoic acid methyl ester from Step A (122 mg, 0.32 mmol) in dichloromethane (2 mL) was added N-bromosuccinimide (57 mg, 0.32 mmol). The solution was stirred at ambient temperature for two hours. The solution was washed with water and brine and dried over magnesium sulfate. The slurry was filtered and concentrated to provide the brominated product as colorless oil (148 mg, quantitative yield). MS (M, M+2): 458, 460

후처리

  1. washThe solution was washed with water and brine
  2. dry with materialdried over magnesium sulfate
  3. filtrationThe slurry was filtered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5b3bdad50aef4b01af29a1c741ad8fbc
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056110B2

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