Reaktion #71745

ord-3540bec67c3547b392f9605095eb2780

Reaktionsgleichung

CC1(C(=O)C(F)(F)F)SCCCS1
2,2,2-Trifluoro-1-(2-methyl-1,3-dithian-2-yl)ethanone
COC(C=O)OC
dimethoxyacetaldehyde
N
ammonia
O=C1CCC(=O)N1Cl
NCS
COC(OC)c1nc(C(F)(F)F)c(C)[nH]1
2-(Dimethoxymethyl)-5-methyl-4-(trifluoromethyl)-1H-imidazole

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONdistilled water (10 mL)
  2. 2
    workup.STIRRINGthe mixture was stirred at room temperature for 18 hours
  3. 3
    FiltrationThe reaction solution was filtered through celite
  4. 4
    Einengenconcentrated under reduced pressure
  5. 5
    SonstigeThe resulting compound was used for the next reaction without purification

Vorschrift

NCS (870 mg, 6.51 mmol) and silver nitrate (1.48 g, 8.71 mmol) were dissolved in acetonitrile (40 mL) and distilled water (10 mL). 2,2,2-Trifluoro-1-(2-methyl-1,3-dithian-2-yl)ethanone obtained in Example (36a) (500 mg, 2.17 mmol) was added, and the mixture was stirred for 40 minutes. Thereafter, dimethoxyacetaldehyde (5.76 M aqueous solution, 0.4 mL, 23.0 mmol) and 28% aqueous ammonia (2 mL) were added, and the mixture was stirred at room temperature for 18 hours. The reaction solution was filtered through celite and then concentrated under reduced pressure. The resulting compound was used for the next reaction without purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536197B2uspto-grants-2013_09