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2,2,2-Trifluoroethanol → Stk076603

HRID 329556
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 329556
[NH2:1][C:2]1[N:7]=[C:6](Cl)[N:5]=[C:4]([NH:9][CH3:10])[N:3]=1.[OH-].[K+].[F:13][C:14]([F:18])([F:17])[CH2:15][OH:16]>>[NH2:1][C:2]1[N:3]=[C:4]([NH:9][CH3:10])[N:5]=[C:6]([O:16][CH2:15][C:14]([F:18])([F:17])[F:13])[N:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 64092,2,2-TrifluoroethanolHCID 14797Potassium HydroxideHCID 2249702-Chloro-4-methylamino-6-amino-1,3,5-triazine-

Produkt 1

HCID 1375559Stk076603

Versuchsvorschrift

2-Amino-4-chloro-6-methylamino-1,3,5-triazine (0.2 mole) was slurried in 80 ml of 2,2,2-trifluoroethanol at room temperature. Potassium hydroxide pellets (0.2 mole) were added portionwise and the mixture was stirred at room temperature overnight. The following day the reaction was heated at gentle reflux for 2 hours during which time the solids gradually dissolved. The solution was cooled and the solvent was removed under vacuum. The residue was washed with water and filtered to give 20.9 g shining off-white crystals of the product named above with the following characteristics: m.p. 204°-205° C. NMR (DMSO-d6): δ2.75, d, (NHCH3); 4.8, q, (OCH2CF3); 6.5-7.3, m, (NH2 +NHCH3).

Aufarbeitung

  1. temperatureThe following day the reaction was heated
  2. temperatureat gentle reflux for 2 hours during which time the solids
  3. dissolutiongradually dissolved
  4. temperatureThe solution was cooled
  5. customthe solvent was removed under vacuum
  6. washThe residue was washed with water
  7. filtrationfiltered
  8. customto give 20.9 g

Quellen und Nachweise

ORD-Eintrag
ord-5a548cd0e5b5472da1299db2530ce1f5
Quelldatensatz
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04892575

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