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Sulfuric Acid → HCID 13013672, 화합물

HRID 2166794
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HRID 2166794 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:10]([F:13])([F:12])[F:11])[CH:5]=[CH:6][C:7]=1[O:8]C.S(=O)(=O)(O)O.[N+:19]([O-])([O-:21])=[O:20].[K+]>ClCCCl>[F:1][C:2]1[CH:3]=[C:4]([C:10]([F:13])([F:12])[F:11])[CH:5]=[C:6]([N+:19]([O-:21])=[O:20])[C:7]=1[OH:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 24434Potassium NitrateHCID 130136742-Fluoro-1-methoxy-4-(trifluoromethyl)benzene

생성물 1

HCID 13013672HCID 13013672, 화합물수율 86.2%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

The product from (c) (4.1 g) in 1,2-dichloro-ethane (25 ml) was chilled to -10° C. and concentrated sulphuric acid (25 ml) added. The mixture was stirred and kept at -5° to -10° C. while potassium nitrate (2.3 g) was added in portions over a period of 30 minutes. The mixture was stirred for a further 30 minutes at below 0° C. and then poured on to ice (150 ml). The mixture was extracted with chloroform (150 ml) and the extracts washed with water (100 ml), dried (MgSO4) and evaporated to give 3-fluoro-4-hydroxy-5-nitrobenzotrifluoride as a pale yellow liquid (4.1 g).

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후처리

  1. additionwas added in portions over a period of 30 minutes
  2. stirringThe mixture was stirred for a further 30 minutes at below 0° C.
  3. extractionThe mixture was extracted with chloroform (150 ml)
  4. washthe extracts washed with water (100 ml)
  5. dry with materialdried (MgSO4)
  6. customevaporated

출처 및 근거

ORD 기록
ord-36ceb8d6a4f34631b19b25d8960009b7
출처 데이터셋
uspto-grants-1983_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04388472

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