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Methylamine → HCID 68490661, Verbindung

HRID 1878024
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1878024
[F:1][C:2]1[CH:29]=[CH:28][C:5]([C:6]([NH:8][CH2:9][C:10]2([C:24]([F:27])([F:26])[F:25])[C:15]3[CH:16]=[C:17]([C:20]([OH:22])=O)[CH:18]=[CH:19][C:14]=3[NH:13][C:12](=[O:23])[O:11]2)=[O:7])=[CH:4][CH:3]=1.C1N=C[N:32](C(N2C=NC=C2)=O)[CH:31]=1.CN>C1COCC1.CN(C=O)C.C(OCC)(=O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([NH:8][CH2:9][C:10]2([C:24]([F:26])([F:25])[F:27])[C:15]3[CH:16]=[C:17]([C:20]([NH:32][CH3:31])=[O:22])[CH:18]=[CH:19][C:14]=3[NH:13][C:12](=[O:23])[O:11]2)=[O:7])=[CH:28][CH:29]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 3

HCID 6329MethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 68486396HCID 68486396, Verbindung

Produkt 1

HCID 68490661HCID 68490661, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6228DimethylformamideLösungsmittelHCID 8028
Tetrahydrofuran
Lösungsmittel
HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

4-{[(4-Fluorobenzoyl)amino]methyl}-2-oxo-4-(trifluoromethyl)-1,4-dihydro-2H-3,1-benzoxazine-6-carboxylic acid (30 mg, 0.073 mmol) and CDI (23.6 mg, 0.15 mmol) were dissolved in THF (230 μL) and DMF (90 μL), and the solution was stirred at room temperature for 30 minutes and thereafter, methylamine (182 μL, 0.36 mmol) was added thereto. The reaction solution was stirred at room temperature for 30 minutes and then diluted with ethyl acetate, which was washed sequentially with water and saturated brine and then dried over magnesium sulfate. After the drying agent was removed by filtration, the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography, whereby the objective compound (10.2 mg, 33%) was obtained as a white solid.

Aufarbeitung

  1. washwas washed sequentially with water and saturated brine
  2. dry with materialdried over magnesium sulfate
  3. customAfter the drying agent was removed by filtration
  4. customthe solvent was evaporated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography, whereby the objective compound (10.2 mg, 33%)
  6. customwas obtained as a white solid

Quellen und Nachweise

ORD-Eintrag
ord-a8a52e79c433407fbda76272eeb0b9cd
Quelldatensatz
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08314094B2

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