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Hydrochloric Acid → [4-(3-Pyrimidylcarboxyamino)-2-phenylbenzoyl]methionine methyl ester

HRID 383126
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 383126
C[O:2][C:3](N1C=CC=NC1)=[O:4].[OH-].[Na+].Cl.Cl.[CH3:15][O:16][C:17](=[O:39])[C@H:18]([CH2:35][CH2:36][S:37][CH3:38])[NH:19][C:20](=[O:34])[C:21]1[CH:26]=[CH:25][C:24]([NH2:27])=[CH:23][C:22]=1[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.ON1C(=O)C2C=CC=CC=2N=N1.CN(C)CC[CH2:56][N:57]=[C:58]=[N:59][CH2:60][CH3:61].C(N(CC)CC)C>C1COCC1.C(OCC)(=O)C>[CH3:15][O:16][C:17](=[O:39])[C@H:18]([CH2:35][CH2:36][S:37][CH3:38])[NH:19][C:20](=[O:34])[C:21]1[CH:26]=[CH:25][C:24]([N:27]([N:57]2[CH:56]=[CH:61][CH:60]=[N:59][CH2:58]2)[C:3]([OH:4])=[O:2])=[CH:23][C:22]=1[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 7

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 730263-hydroxy-1,2,3-benzotriazin-4(3H)-oneHCID 69612387(4-Amino-2-phenylbenzoyl)methionine methyl ester hydrochloride2×
HCID 70212497
3-Pyrimidinecarboxylic acid methyl ester

Produkt 1

HCID 69845184[4-(3-Pyrimidylcarboxyamino)-2-phenylbenzoyl]methionine methyl esterAusbeute 41 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A mixture of the 5-pyrimidinecarboxylic acid methyl ester prepared in Example 219A (682 mg, 4.94 mmol) and aqueous sodium hydroxide solution (4.0 M, 2.5 mL) in THF was heated at 60° C. for 1.5 hours. Hydrochloric acid (6.0 N, 2 mL) was added to the reaction mixture, and the solvent was evaporated in vacuo. The residue was dried under high vacuum at 50° C. for 1 hour, and the redesolved in to THF. To the acid solution was added (4-amino-2-phenylbenzoyl)methionine methyl ester (compound 8, 1.97 g, 5.0 mmol), 3-hydroxy 1,2,3-benzotriazin-4(3H)-one (0.978 g, 6.0 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (1.15 g, 6.0 mmol) and triethylamine (2.8 mL, 20 mmol). After 14 hours, the reaction mixture was diluted with ethyl acetate (100 mL), washed with water and brine, dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The residue was then purified by column chromatography (50% ethyl acetate-hexane, then ethyl acetate) to give [4-(3-pyrimidylcarboxyamino)-2-phenylbenzoyl]methionine methyl ester (0.937 g, 41%).

Aufarbeitung

  1. customthe solvent was evaporated in vacuo
  2. customThe residue was dried under high vacuum at 50° C. for 1 hour
  3. washwashed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was then purified by column chromatography (50% ethyl acetate-hexane

Quellen und Nachweise

ORD-Eintrag
ord-5ffb306a633444b48646a6b11235b4b1
Quelldatensatz
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06310095B1

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