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Ethanol, 2-chloro-, 1-(4-methylbenzenesulfonate) → HCID 58396201, 화합물

HRID 446258
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HRID 446258 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([OH:14])[CH:7]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:9]=1)([O-])=O.C(=O)([O-])[O-].[Cs+].[Cs+].C1(C)C=CC(S(O[CH2:31][CH2:32][Cl:33])(=O)=O)=CC=1>O>[Cl:33][CH2:32][CH2:31][O:14][C:6]1[CH:5]=[C:4]([NH2:1])[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6639Ethanol, 2-chloro-, 1-(4-methylbenzenesulfonate)HCID 10796Cesium carbonateHCID 27562513-Hydroxy-5-nitrobenzotrifluoride

생성물 1

HCID 58396201HCID 58396201, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 3-nitro-5-(trifluoromethyl)phenol (2.10 g, 10.1 mmol) and cesium carbonate (4.00 g, 12.2 mmol) in acetonenitrile (50 ml) was added 2-chloroethyl p-toluenesulfonate (2.9 g, 12 mmol) slowly. The resulting mixture was stirred at RT for 5 hr, poured into water (100 ml) and then extracted with EtOAc (3×80 ml). The combined organic layer was washed with brine (100 ml) and dried over Na2SO4. Solvent was removed under vacuum and the residue was purified by flash column chromatography on the silica gel (hexane/EtOAc=5 to 25%) to afford the desired compound.

후처리

  1. extractionextracted with EtOAc (3×80 ml)
  2. washThe combined organic layer was washed with brine (100 ml)
  3. dry with materialdried over Na2SO4
  4. customSolvent was removed under vacuum
  5. customthe residue was purified by flash column chromatography on the silica gel (hexane/EtOAc=5 to 25%)

출처 및 근거

ORD 기록
ord-633a84f13fa5495885a16e8147de5568
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08476434B2

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