Potassium Carbonate → HCID 21877064, 화합물

HRID 723626노트

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HRID 723626 반응식
C(=O)([O-])[O-].[K+].[K+].[Br:7][C:8]1[CH:9]=[C:10]([SH:15])[CH:11]=[C:12]([Br:14])[CH:13]=1.Cl[CH:17]([C:22](=[O:25])[CH2:23][CH3:24])[C:18](=[O:21])[CH2:19][CH3:20]>CC(C)=O>[Br:7][C:8]1[CH:9]=[C:10]([S:15][CH:17]([C:22](=[O:25])[CH2:23][CH3:24])[C:18](=[O:21])[CH2:19][CH3:20])[CH:11]=[C:12]([Br:14])[CH:13]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 218770573,5-Dibromobenzene-1-thiolHCID 218770754-Chloroheptane-3,5-dione

생성물 1

HCID 21877064HCID 21877064, 화합물수율 72.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Potassium carbonate (1.9 g, 14 mmol) was added to a solution of 3,5-dibromobenzenethiol (2.84 g, 10.5 mmol) (Preparation 48) and 4-chloroheptane-3,5-dione (1.7 g, 10.5 mmol) (Preparation 40) in acetone (12 ml) producing a white suspension. The mixture was stirred at room temperature for 15 hours. The mixture was concentrated under reduced pressure and the residue was partitioned between dichloromethane (100 ml) and 1N hydrochloric acid (70 ml). The aqueous layer was extracted with further dichloromethane (2×100 ml). The combined organic layers were washed with brine (50 ml), dried over magnesium sulphate, filtered and concentrated under reduced pressure to leave a pink oil. The crude product was purified by flash chromatography on silica gel eluting with pentane:dichloromethane (1:1, by volume) to provide the title compound (3 g) as a pink oil.

후처리

  1. customproducing a white suspension
  2. concentrationThe mixture was concentrated under reduced pressure
  3. customthe residue was partitioned between dichloromethane (100 ml) and 1N hydrochloric acid (70 ml)
  4. extractionThe aqueous layer was extracted with further dichloromethane (2×100 ml)
  5. washThe combined organic layers were washed with brine (50 ml)
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customto leave a pink oil
  10. customThe crude product was purified by flash chromatography on silica gel eluting with pentane:dichloromethane (1:1, by volume)

출처 및 근거

ORD 기록
ord-8ae2888357c743c898e2175234824155
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07141585B2

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