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Nitroethane → 1-Methanesulfonyl-4-(2-nitro-propenyl)-2-trifluoromethyl-benzene

HRID 908191
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반응식

HRID 908191 반응식
[CH3:1][S:2]([C:5]1[CH:12]=[CH:11][C:8]([CH:9]=O)=[CH:7][C:6]=1[C:13]([F:16])([F:15])[F:14])(=[O:4])=[O:3].[N+:17]([CH2:20][CH3:21])([O-:19])=[O:18].C([O-])(=O)C.[NH4+]>ClCCl>[CH3:1][S:2]([C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[C:20]([N+:17]([O-:19])=[O:18])[CH3:21])=[CH:7][C:6]=1[C:13]([F:16])([F:15])[F:14])(=[O:4])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6587NitroethaneHCID 517165Ammonium AcetateHCID 714799064-Methanesulfonyl-3-trifluoromethyl-benzaldehyde

생성물 1

HCID 673913281-Methanesulfonyl-4-(2-nitro-propenyl)-2-trifluoromethyl-benzene

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A stirred mixture of 4-methanesulfonyl-3-trifluoromethyl-benzaldehyde (Example 5001a) (12 g, 47 mmol), nitroethane (27.5 ml, 380 mol) and ammonium acetate (1.22 g, 16 mmol) is heated at reflux under argon for 18 hours. The mixture is concentrated to give an oil which is dissolved in dichloromethane (200 ml) and washed with water (3×200 ml), followed by brine (200 ml). The organic extract is dried (MgSO4), filtered and the solvent removed to give the product as red oil. This is used immediately in the next step.

후처리

  1. temperatureis heated
  2. temperatureat reflux under argon for 18 hours
  3. concentrationThe mixture is concentrated
  4. customto give an oil which
  5. washwashed with water (3×200 ml)
  6. extractionThe organic extract
  7. dry with materialis dried (MgSO4)
  8. filtrationfiltered
  9. customthe solvent removed

출처 및 근거

ORD 기록
ord-bbebb2d3796b4798bf0cc7e489898e26
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08017608B2

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