Iodine → HCID 57428844, 화합물

HRID 507619노트

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HRID 507619 반응식
II.[PH2](O)=O.[F:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([C:16]2[S:17][CH:18]=[CH:19][N:20]=2)(O)[CH3:14])=[CH:9][CH:8]=1.[OH-].[Na+]>C(O)(=O)C>[F:6][C:7]1[CH:12]=[CH:11][C:10]([CH:13]([C:16]2[S:17][CH:18]=[CH:19][N:20]=2)[CH3:14])=[CH:9][CH:8]=1

참가 물질

6

반응물 4

HCID 807IodineHCID 14798Sodium HydroxideHCID 4124402Phosphinic AcidHCID 57428843HCID 57428843, 화합물

생성물 1

HCID 57428844HCID 57428844, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
60 °C

실험 절차

A mixture of iodine (856 mg, 3.37 mmol), hypophosphorous acid (3.152 mL, 20.22 mmol) and acetic acid (40 mL) was heated to 60° C. until the reaction mixture became clear. 1-(4-fluorophenyl)-1-(thiazol-2-yl)ethanol (1.05 g, 5.07 mmol) was added to the solution and the reaction mixture was heated to 80° C. overnight. After cooling to rt, the reaction mixture was neutralized with concentrated sodium hydroxide and the crude product was extracted with chloroform, washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The crude product was purified by flash chromatography with 0-40% ethyl acetate in hexane to afford the title compound as an oily brown residue (351 mg, 50% yield). MS (M+H)+ 208.

후처리

  1. temperaturethe reaction mixture was heated to 80° C. overnight
  2. temperatureAfter cooling to rt
  3. extractionthe crude product was extracted with chloroform
  4. washwashed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe crude product was purified by flash chromatography with 0-40% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-99a43512c9f24fa7854078f0ffafd8db
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786132B2

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