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Water → Methyl-phenyl-carbamic Acid 5-(4-methoxy-phenoxy)-pyrimidin-2-yl Ester

HRID 1831252
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HRID 1831252 반응식
[CH3:1][O:2][C:3]1[CH:16]=[CH:15][C:6]([O:7][C:8]2[CH:9]=[N:10][C:11]([OH:14])=[N:12][CH:13]=2)=[CH:5][CH:4]=1.[CH3:17][N:18]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:19](Cl)=[O:20].N12CCN(CC1)CC2.O>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:16]=[CH:15][C:6]([O:7][C:8]2[CH:9]=[N:10][C:11]([O:14][C:19](=[O:20])[N:18]([CH3:17])[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[N:12][CH:13]=2)=[CH:5][CH:4]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 9237DabcoHCID 77969Carbamic chloride, N-methyl-N-phenyl-HCID 178492489HCID 178492489, 화합물

생성물 1

HCID 69519671Methyl-phenyl-carbamic Acid 5-(4-methoxy-phenoxy)-pyrimidin-2-yl Ester수율 79%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

A solution of 5-(4-methoxy-phenoxy)-pyrimidin-2-ol (0.44 g, 2.00 mmol), N-methyl-N-phenylcarbamoyl chloride (0.34 g, 2.00 mmol) and 1,4-diazabicyclo[2.2.2]octane (0.22 g, 2.00 mmol) in dimethylformamide (15 ml) was stirred at room temperature for 1 hour. Water was added and the precipitates were collected by suction. The solids were dissolved in dichloromethane and the solution was dried over sodium sulphate, filtered and evaporated in vacuo. The residue was crystallised from ethyl acetate:heptane yielding the title compound (0.55 g, 79% yield) as an off-white solid.

후처리

  1. customthe precipitates were collected by suction
  2. dissolutionThe solids were dissolved in dichloromethane
  3. dry with materialthe solution was dried over sodium sulphate
  4. filtrationfiltered
  5. customevaporated in vacuo
  6. customThe residue was crystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-c77f3327d0ec4f45963a5402eeeebf45
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07067517B2

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