StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Hydrochloric Acid → 6-Benzyl-4,5,6,7,7a,8-hexahydro-3bH-3-thia-6-aza-cyclopenta[alpha]indene

HRID 30280
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 30280
[Al+3].[Cl-].[Cl-].[Cl-].C(NB)(C)(C)C.[CH2:11]([N:18]1[CH2:26][CH2:25][CH:24]2[CH:20]([C:21](=O)[C:22]3[CH:29]=[CH:28][S:27][C:23]=32)[CH2:19]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Al+3].[Cl-].[Cl-].[Cl-].B.Cl.[OH-].[Na+]>C(Cl)Cl>[CH2:11]([N:18]1[CH2:26][CH2:25][CH:24]2[CH:20]([CH2:21][C:22]3[CH:29]=[CH:28][S:27][C:23]=32)[CH2:19]1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 6

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 3639180N-boranyl-2-methylpropan-2-amineHCID 6451240Aluminum(III) ChlorideHCID 597894266-Benzyl-3b,4,5,6,7,7a-hexahydro-3-thia-6-aza-cyclopenta[alpha]inden-8-oneHCID 178419134HCID 178419134, Verbindung

Produkt 1

HCID 1317270426-Benzyl-4,5,6,7,7a,8-hexahydro-3bH-3-thia-6-aza-cyclopenta[alpha]indeneAusbeute 62 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A slurry of AlCl3 (2.74 g, 20.76 mmol) in CH2Cl2 (21 ml) was treated with tert-butylaminoborane (3.57 g, 41.52 mmol) at 0° C. and stirred for 30 minutes. Next, a solution of the product from step e) (1.96 g, 6.92 mmol) in CH2Cl2 (15 ml) was added dropwise to the AlCl3/borane solution. After 2 hours at 0° C., the crude reaction mixture was poured into cold 10% HCl, treated with 2 M NaOH to pH 12 and extracted with CH2Cl2 (3×75 ml). The combined organic extracts were washed with brine (75 ml), dried (MgSO4), and the solvent evaporated in vacuo leaving the crude product that was purified by silica-gel chromatography using a ethyl acetate/hexanes gradient (0% to 75% ethyl acetate) to give 1.16 g (62%) of the subtitle compound. MS calculated for C17H19NS+H 270, observed 270.

Aufarbeitung

  1. waitAfter 2 hours at 0° C.
  2. customthe crude reaction mixture
  3. extractionextracted with CH2Cl2 (3×75 ml)
  4. washThe combined organic extracts were washed with brine (75 ml)
  5. dry with materialdried (MgSO4)
  6. customthe solvent evaporated in vacuo
  7. customleaving the crude product that
  8. customwas purified by silica-gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-9aed20561ff2423b8a1e7d3354d14eca
Quelldatensatz
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07423056B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion