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Sulfuric Acid → HCID 17930983, 화합물

HRID 900439
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HRID 900439 반응식
[NH2:1][C:2]1[S:3][C:4]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:5]([C:9]([F:12])([F:11])[F:10])[C:6]=1[C:7]#[N:8].S(=O)(=O)(O)[OH:20].C(=O)(O)[O-].[Na+]>>[NH2:1][C:2]1[S:3][C:4]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:5]([C:9]([F:10])([F:12])[F:11])[C:6]=1[C:7]([NH2:8])=[O:20]
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참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 179309512-Amino-5-phenyl-4-(trifluoromethyl)-3-thiophenecarbonitrile

생성물 1

HCID 17930983HCID 17930983, 화합물

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온도
50 °C

실험 절차

A mixture of 2-amino-4-trifluoromethyl-5-phenyl-3-thiophenenitrile (0.12 g) and concentrated sulphuric acid (1.5 ml) was stirred and heated at 50° C. for 8 h. The reaction mixture was added to saturated aqueous sodium bicarbonate until a pH of 7 was obtained. The product was extracted into ethyl acetate (100 ml) and the organic layer was dried with anhydrous sodium sulfate (3 g), filtered and concentrated. The residue was chromatographed on silica gel eluting with ethyl acetate/isohexane mixtures. The solvent was removed and the product collected (0.07 g).

후처리

  1. customwas obtained
  2. extractionThe product was extracted into ethyl acetate (100 ml)
  3. dry with materialthe organic layer was dried with anhydrous sodium sulfate (3 g)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel eluting with ethyl acetate/isohexane mixtures
  7. customThe solvent was removed
  8. customthe product collected (0.07 g)

출처 및 근거

ORD 기록
ord-eb6ef6370da04431a0d42e3242612ebb
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07358376B2

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