반응 #71745

ord-3540bec67c3547b392f9605095eb2780

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536197B2uspto-grants-2013_09