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Triethylsilane → methyl 6-benzyl-4-cyclohexyl-5-phenyl-6H-thieno[2,3-b]pyrrole-2-carboxylate

HRID 505826
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 505826
[CH2:1]([N:8]1[C:12]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:11]([C:19]2[CH2:24][CH2:23][CH2:22][CH2:21][CH:20]=2)[C:10]2[CH:25]=[C:26]([C:28]([O:30][CH3:31])=[O:29])[S:27][C:9]1=2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([SiH](CC)CC)C>C(O)(C(F)(F)F)=O>[CH2:1]([N:8]1[C:12]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:11]([CH:19]2[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24]2)[C:10]2[CH:25]=[C:26]([C:28]([O:30][CH3:31])=[O:29])[S:27][C:9]1=2)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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Komponenten

4

Edukt 2

HCID 12052TriethylsilaneHCID 68467568methyl 6-benzyl-4-cyclohex-1-en-1-yl-5-phenyl-6H-thieno[2,3-b]pyrrole-2-carboxylate

Produkt 1

HCID 11441793methyl 6-benzyl-4-cyclohexyl-5-phenyl-6H-thieno[2,3-b]pyrrole-2-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution (0.7 M) of methyl 6-benzyl-4-cyclohex-1-en-1-yl-5-phenyl-6H-thieno[2,3-b]pyrrole-2-carboxylate in TFA at 0° C. was treated with triethylsilane (1.5 eq.). The mixture was stirred at 0° C. for 1 h then concentrated to give a residue that was purified by flash chromatography on silica gel (1:30 acetone/toluene) affording methyl 6-benzyl-4-cyclohexyl-5-phenyl-6H-thieno[2,3-b]pyrrole-2-carboxylate as a solid that was dissolved in THF/MeOH (1:1). The resulting solution (0.04 M) was treated with aqueous KOH (1 N solution, 4 eq.) then the mixture was heated to 80° C. for 4 h. After cooling down, the mixture was concentrated then the resulting residue was diluted with water and pH was turned to neutral value by addition of aqueous ammonium chloride (saturated solution). The mixture was concentrated to give a residue that was purified by RP-HPLC (Conditions: Waters X-TERRA MS C18, 10 micron, 10×150 mm; flow: 20 mL/min; Gradient: A: H2O+0.05% TFA; B: MeCN+0.05% TFA; 50% A isocratic for 2 min then linear to 0% A in 10 min) to afford the title compound (58%) as a solid.

Aufarbeitung

  1. concentrationthen concentrated
  2. customto give a residue that
  3. customwas purified by flash chromatography on silica gel (1:30 acetone/toluene)

Quellen und Nachweise

ORD-Eintrag
ord-76094b2f22074027acf6eb6ba540df58
Quelldatensatz
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07781431B2

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