Methyl iodide → Methyl 3-bromo-4-(pyrrolidin-1-ylcarbonyl)benzoate

HRID 2053762노트

반응식

HRID 2053762 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[C:11]([N:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1)=[O:12])[C:5]([OH:7])=[O:6].[C:18](=O)([O-])[O-].[Cs+].[Cs+].IC>CN(C)C=O>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[C:11]([N:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1)=[O:12])[C:5]([O:7][CH3:18])=[O:6]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 693124883-Bromo-4-(pyrrolidin-1-ylcarbonyl)benzoic acid

생성물 1

HCID 69312594Methyl 3-bromo-4-(pyrrolidin-1-ylcarbonyl)benzoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

20 g (67.1 mmol) of 3-bromo-4-(pyrrolidin-1-ylcarbonyl)benzoic acid is dissolved in 400 mL of N,N-dimethylformamide and combined with 21.9 g (67.1 mmol) cesium carbonate with stirring. Then 4.21 mL (67.1 mmol) of iodomethane is slowly added dropwise at ambient temperature and the mixture is stirred for 16 hours at ambient temperature. After the solid constituents have been removed by filtration with suction, volatile constituents are removed in vacuo. Yield: 20.94 g (75%); Rf value: 0.42 (silica gel; dichloromethane/ethanol=98:2); C13H14BrNO3 (312.17); mass spectrum: (M+H)+=312/314 (bromine isotope).

후처리

  1. stirringthe mixture is stirred for 16 hours at ambient temperature
  2. customAfter the solid constituents have been removed by filtration with suction, volatile constituents
  3. customare removed in vacuo

출처 및 근거

ORD 기록
ord-1f631f885c4c4dd887240ea6ca9a1da1
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07326791B2

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