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Hydrochloric Acid → (4-Nitro-2-phenylbenzoyl)methionine 2-trimethylsilylethyl ester

HRID 2121222
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2121222
[CH3:1][O:2][C:3](=[O:27])[C@H:4]([CH2:23][CH2:24][S:25][CH3:26])[NH:5][C:6](=[O:22])[C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][C:8]=1[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[OH-].[Li+].Cl.[CH3:31][Si:32]([CH3:37])([CH3:36])[CH2:33]CO.C(N=C=NC(C)C)(C)C>CO.CN(C)C1C=CN=CC=1.C1COCC1>[CH3:31][Si:32]([CH3:37])([CH3:36])[CH2:33][CH2:1][O:2][C:3](=[O:27])[C@H:4]([CH2:23][CH2:24][S:25][CH3:26])[NH:5][C:6](=[O:22])[C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][C:8]=1[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 313Hydrochloric Acid2×HCID 3939Lithium HydroxideHCID 12734DiisopropylcarbodiimideHCID 180132-(Trimethylsilyl)ethanolHCID 18666764(4-Nitro-2-phenylbenzoyl)methionine methyl ester

Produkt 1

HCID 69844218
(4-Nitro-2-phenylbenzoyl)methionine 2-trimethylsilylethyl ester
Ausbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of (4-nitro-2-phenylbenzoyl)methionine methyl ester (7.69 g, 30 mmol), prepared as in Example 192A and aqueous saturated lithium hydroxide (20 mL) in methanol (50 mL) was refluxed for 6 hours. The reaction mixture was carefully acidified with concentrated hydrochloric acid (10 mL), and extracted with ethyl acetate (4×). The combine extracts were washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was dissolved in dichloromethane (50 mL) and THF (10 mL) and 2-trimethylsilylethanol (3.72 g, 31.5 mmol), 1,3-diisopropylcarbodiimide (5.17 mL, 33 mmol) and 4-dimethylaminopyridine (30 mg) were added sequentially. After 4 hours, aqueous hydrochloric acid (0.1 N, 0.5 mL) was added and the reaction mixture was stirred for another 2 hours. The reaction mixture was then filtered through silica gel (40 g), and the filtrate was concentrated in vacuo. The residue was purified by column chromatography (5% ethyl ether-hexane) to give the title compound (8.90 g, 87%).

Aufarbeitung

  1. temperaturewas refluxed for 6 hours
  2. extractionextracted with ethyl acetate (4×)
  3. washThe combine extracts were washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. dissolutionThe residue was dissolved in dichloromethane (50 mL)
  8. filtrationThe reaction mixture was then filtered through silica gel (40 g)
  9. concentrationthe filtrate was concentrated in vacuo
  10. customThe residue was purified by column chromatography (5% ethyl ether-hexane)

Quellen und Nachweise

ORD-Eintrag
ord-c9352c20a5d0439eb70d4779182299fe
Quelldatensatz
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06693123B2

Notizen zur Reaktion

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