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

HRID 2103612
ノート
印刷プレビュー

反応式

HRID 2103612 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 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)-propenal2 回

生成物 1

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

試薬・触媒・溶媒 4

HCID 11979704Tetrakis(triphenylphosphine)palladium触媒HCID 887Methanol溶媒2 回HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c276c70d98de4eefae9c4998267d41a7
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07576108B2

反応ノート

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