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Cesium fluoride → (Z)-3-Cyclohexyl-2-(5-methanesulfonyl-thiophen-2-yl)-prop-2-en-1-ol

HRID 2103612
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HRID 2103612 반응식
BrC1SC(S(C)(=O)=O)=CC=1.[F-].[Cs+].C1(C=C(B2OC(C)(C)C(C)(C)O2)CO)CCCCC1.[CH:32]1(/[CH:38]=[C:39](\[C:42]2[S:43][C:44]([S:47]([CH3:50])(=[O:49])=[O:48])=[CH:45][CH:46]=2)/[CH:40]=[O:41])[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]1.[BH4-].[Na+]>O1CCOCC1.CO.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O>[CH:32]1(/[CH:38]=[C:39](\[C:42]2[S:43][C:44]([S:47]([CH3:50])(=[O:49])=[O:48])=[CH:45][CH:46]=2)/[CH2:40][OH:41])[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]1
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참가 물질

10

반응물 5

HCID 25953Cesium fluorideHCID 4311764Sodium borohydrideHCID 173902812-Bromo-5-methanesulfonylthiopheneHCID 670845993-Cyclohexyl-2-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-prop-2-en-1-olHCID 86605125(Z)-3-cyclohexyl-2-(5-methanesulfonyl-thiophen-2-yl)-propenal2회

생성물 1

HCID 69058010
(Z)-3-Cyclohexyl-2-(5-methanesulfonyl-thiophen-2-yl)-prop-2-en-1-ol

시약·촉매·용매 4

HCID 11979704Tetrakis(triphenylphosphine)palladium촉매HCID 887Methanol용매2회HCID 962Water용매2회HCID 312751,4-Dioxane용매

반응 조건

온도
80 °C

실험 절차

Add 2-bromo-5-methanesulfonyl-thiophene (2.26 g, 9.39 mmol), caesium fluoride ( 2.85 g, 18.78 mmol) and tetrakis-(triphenylphosphin)-palladium(0) (543 mg, 0.47 mmol) to a solution of 3-cyclohexyl-2-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-prop-2-en-1-ol (2.5 g, 9.39 mmol) in dioxane (50 mL). Stir at 80° C. for 24 h, monitor completion of the reaction by LCMS. Treat the reaction mixture with water and extract with dichloromethane. Dry organic layers over sodium sulfate and remove solvents under vacuum to obtain 4.85 g crude product. Purify by siliga gel chromatography, eluting with gradient from 10:0 to 7:3 hexane:ethyl acetate. 690 mg isolated product was (Z)-3-cyclohexyl-2-(5-methanesulfonyl-thiophen-2-yl)-propenal. MS (m/e): 299.0 (M+H). Add a solution of (Z)-3-cyclohexyl-2-(5-methanesulfonyl-thiophen-2-yl)-propenal (690 mg, 2.31 mmol) in methanol (2 mL) to a suspension of NaBH4 in methanol (3 mL) at 0° C. and stir for 1 h, monitor completion of the reaction by LCMS. Dilute reaction mixture with water, extract with ethyl acetate, wash combined organic layers with water and saturated sodium chloride, dry over sodium sulfate and remove solvent under vacuum to obtain 704 mg crude product. MS (m/e): 301.0 (M+H).

후처리

  1. customcompletion of the reaction by LCMS
  2. extractionextract with dichloromethane
  3. customDry organic layers over sodium sulfate and remove solvents under vacuum
  4. customto obtain 4.85 g crude product
  5. customPurify by siliga gel chromatography
  6. washeluting with gradient from 10:0 to 7:3 hexane
  7. custom690 mg isolated product
  8. stirringstir for 1 h
  9. customcompletion of the reaction by LCMS
  10. additionDilute
  11. extractionextract with ethyl acetate
  12. washwash
  13. dry with materialdry over sodium sulfate
  14. customremove solvent under vacuum

출처 및 근거

ORD 기록
ord-c276c70d98de4eefae9c4998267d41a7
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576108B2

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