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Methanol → 1-Chloro-5-fluoro-2-methoxy-4-nitrobenzene

HRID 51444
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HRID 51444 반응식
C(=O)([O-])OCC[C:5]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([F:14])=[CH:7][C:6]=1[Cl:15].[C:18](=O)([O-])[O-:19].[Cs+].[Cs+].IC.CO>CN(C)C=O.O>[Cl:15][C:6]1[CH:7]=[C:8]([F:14])[C:9]([N+:11]([O-:13])=[O:12])=[CH:10][C:5]=1[O:19][CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 887MethanolHCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 66588385(2-Chloro-4-fluoro-5-nitrophenyl)-ethyl carbonate

생성물 1

HCID 27792951-Chloro-5-fluoro-2-methoxy-4-nitrobenzene수율 97.1%

시약·촉매·용매 2

HCID 962Water용매HCID 6228

실험 절차

A solution of 15.0 g of (2-chloro-4-fluoro-5-nitrophenyl)-ethyl carbonate in 100 ml of dimethyl formamide was treated with 18.6 g of cesium carbonate, 7.1 ml of iodomethane and 7 ml of methanol and stirred overnight at room temperature. The reaction mixture was poured into water and extracted twice with ether. The extracts were washed twice with water and then with brine, dried over magnesium sulfate and concentrated to afford 11.4 g of the subtitle compound. mp. 69-70° C. Ex. 57, C.

후처리

  1. extractionextracted twice with ether
  2. washThe extracts were washed twice with water
  3. dry with materialwith brine, dried over magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-faa14b06cf2b4e0d9eae0409f8197195
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06713645B1

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Dimethylformamide
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