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Potassium Dichromate → HCID 11323174, 화합물

HRID 1099425
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HRID 1099425 반응식
[F:1][C:2]([F:16])([F:15])[S:3]([O:6][C:7]1[CH:14]=[CH:13][C:10]([CH:11]=[O:12])=[CH:9][CH:8]=1)(=[O:5])=[O:4].[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=[O:18].[K+].[K+]>S(=O)(=O)(O)O>[F:16][C:2]([F:15])([F:1])[S:3]([O:6][C:7]1[CH:14]=[CH:13][C:10]([C:11]([OH:18])=[O:12])=[CH:9][CH:8]=1)(=[O:4])=[O:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24502Potassium DichromateHCID 108796304-(Trifluoromethanesulfonyloxy)benzaldehyde

생성물 1

HCID 11323174HCID 11323174, 화합물수율 114.5%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
65 °C

실험 절차

A suspension of 4-(trifluoromethanesulfonyloxy)benzaldehyde (5.2 g, 20.5 mmol, described in JACS, 1987, 109, 5478) and potassium dichromate (2.5 g) in sulfuric acid (30%, 47 mL) was heated at 65° C. for 1 h. The mixture was allowed to cool to ambient temperature and then poured on ice. The formed precipitate was filtered off and washed with several portions of water. The crude product was recrystallized from water/ethanol (1:1) affording 2.63 g (47% yield) of the title compound: mp 178-180° C.; 1H NMR (400 MHz, DMSO-d6) δ 8.11 (d, 2 H), 7.64 (d, 2 H).

후처리

  1. temperatureto cool to ambient temperature
  2. additionpoured on ice
  3. filtrationThe formed precipitate was filtered off
  4. washwashed with several portions of water
  5. customThe crude product was recrystallized from water/ethanol (1:1)

출처 및 근거

ORD 기록
ord-bb38fb584f234dfe959df0e7025f3b6c
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08143408B2

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