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Methane → HCID 58372871, 화합물

HRID 888471
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HRID 888471 반응식
[CH2:1]([O:3][C:4](=[O:31])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([O:14][C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-])=O)=[CH:17][C:16]=2[CH2:24][S:25][CH2:26][C:27]([F:30])([F:29])[F:28])[CH:7]=1)[CH3:2].CN(C)N.C>CCO>[CH2:1]([O:3][C:4](=[O:31])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([O:14][C:15]2[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][C:16]=2[CH2:24][S:25][CH2:26][C:27]([F:28])([F:29])[F:30])[CH:7]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 297MethaneHCID 59761,1-DimethylhydrazineHCID 58372816HCID 58372816, 화합물

생성물 1

HCID 58372871HCID 58372871, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of {4-methoxy-3-[4-nitro-2-(2,2,2-trifluoro-ethylsulfanylmethyl)-phenoxy]-phenyl}-acetic acid ethyl ester (1.46 g, 3.18 mmol), ferric chloride (0.026 g, 0.16 mmol), 1,1-dimethylhydrazine (1.69 mL, 22.27 mmol), and DARCO (0.300 g) in EtOH (30 mL) was stirred overnight at 65° C. The mixture was partitioned between EtOAc and H2O and extracted three times with EtOAc. The combined organic layers were washed with H2O and brine, and then dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel chromatography (EtOAc in hexanes gradient) to give the title compound.

후처리

  1. customThe mixture was partitioned between EtOAc and H2O
  2. extractionextracted three times with EtOAc
  3. washThe combined organic layers were washed with H2O and brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel chromatography (EtOAc in hexanes gradient)

출처 및 근거

ORD 기록
ord-d26be22312da46f89b13bf449f1485a3
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08247602B2

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