Triethylamine → 3,6-dichloro-N-[4-(dimethylphosphoryl)phenyl]-1,2,4-triazin-5-amine

HRID 921442Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 921442
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([P:8](=[O:11])([CH3:10])[CH3:9])=[CH:4][CH:3]=1.[Cl:12][C:13]1[N:14]=[N:15][C:16]([Cl:20])=[C:17](Cl)[N:18]=1.C(N(CC)CC)C>C(Cl)Cl>[Cl:12][C:13]1[N:14]=[N:15][C:16]([Cl:20])=[C:17]([NH:1][C:2]2[CH:3]=[CH:4][C:5]([P:8]([CH3:9])([CH3:10])=[O:11])=[CH:6][CH:7]=2)[N:18]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 122624033,5,6-Trichloro-1,2,4-triazineHCID 206345534-(Dimethylphosphoryl)aniline

Produkt 1

HCID 866688243,6-dichloro-N-[4-(dimethylphosphoryl)phenyl]-1,2,4-triazin-5-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of 4-amino-dimethylphenylphosphine oxide (1.6 mmol) and 3,5,6-trichloro-1,2,4-triazine (1.6 mmol) in CH2Cl2, is added triethylamine (2 mmol). The reaction mixture is allowed to cool to room temperature, dissolved in dichloromethane and washed with an aqueous solution of Na2CO3. The dichloromethane extract is dried over MgSO4 and evaporated. The crude product is purified by Prep-HPLC.

Aufarbeitung

  1. washwashed with an aqueous solution of Na2CO3
  2. extractionThe dichloromethane extract
  3. dry with materialis dried over MgSO4
  4. customevaporated
  5. customThe crude product is purified by Prep-HPLC

Quellen und Nachweise

ORD-Eintrag
ord-3bb4ab4281fb4fa0a51077bdc4b022c2
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09273077B2

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