Isopropylamine → HCID 18446929, Verbindung

HRID 1983072Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1983072
[CH:1]([NH2:4])([CH3:3])[CH3:2].[Cl:5][C:6]1[C:7]([N:12]2[C:16]([C:17]3[O:22][C:21](=[O:23])[C:20]4[CH:24]=[C:25]([N+:29]([O-:31])=[O:30])[CH:26]=[C:27]([CH3:28])[C:19]=4[N:18]=3)=[CH:15][C:14]([C:32]([F:35])([F:34])[F:33])=[N:13]2)=[N:8][CH:9]=[CH:10][CH:11]=1>O1CCOCC1>[Cl:5][C:6]1[C:7]([N:12]2[C:16]([C:17]([NH:18][C:19]3[C:20]([C:21]([NH:4][CH:1]([CH3:3])[CH3:2])=[O:23])=[CH:24][C:25]([N+:29]([O-:31])=[O:30])=[CH:26][C:27]=3[CH3:28])=[O:22])=[CH:15][C:14]([C:32]([F:35])([F:34])[F:33])=[N:13]2)=[N:8][CH:9]=[CH:10][CH:11]=1

Komponenten

4

Edukt 2

HCID 6363IsopropylamineHCID 690644832-[1-(3-Chloro-2-pyridinyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl]-8-methyl-6-nitro-4H-3,1-benzoxazin-4-one

Produkt 1

HCID 18446929HCID 18446929, VerbindungAusbeute 14,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Isopropyl amine (0.35 mL, 4.11 mmol) was added to a solution of 619 mg (1.37 mmol) of the product of Step B in dioxane (8 mL) at 25° C. After being stirred overnight, the resulting heterogenous mixture was concentrated and the residue was triturated with methanol (10 mL). Filtration gave 100 mg of the title product. The filtrate was concentrated and the resulting residue was triturated with diethyl ether. Filtration of the resulting solid provided an additional 320 mg of the title product, m.p. 170-172° C.

Aufarbeitung

  1. concentrationthe resulting heterogenous mixture was concentrated
  2. customthe residue was triturated with methanol (10 mL)
  3. filtrationFiltration

Quellen und Nachweise

ORD-Eintrag
ord-884240302a6a4e819bbe11983f6cd039
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07541377B2

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