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Hydrochloric Acid → 2(R)-Amino-5-phenyl-pentanoic acid (2(S)-hydroxy-1(S)-methyl-2-phenyl-ethyl)-methyl-amide

HRID 1068834
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1068834
[CH3:1][CH:2]([N:11]([C:13]([CH2:15][NH2:16])=[O:14])[CH3:12])[CH:3]([OH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[Li+].[Cl-].[Li]CCCC.[C:24]1([CH2:30][CH2:31][CH2:32]Br)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.Cl>C1COCC1.CCOC(C)=O>[OH:10][C@@H:3]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[C@@H:2]([N:11]([CH3:12])[C:13](=[O:14])[C@H:15]([NH2:16])[CH2:32][CH2:31][CH2:30][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[CH3:1]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 12503(3-Bromopropyl)benzeneHCID 433294Lithium ChlorideHCID 44543862-amino-N-(1-hydroxy-1-phenylpropan-2-yl)-N-methylacetamideHCID 178418339Butyllithium

Produkt 1

HCID 53699985
2(R)-Amino-5-phenyl-pentanoic acid (2(S)-hydroxy-1(S)-methyl-2-phenyl-ethyl)-methyl-amide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

A solution of pseudoephedrine glycinamide (1.5 g, 6.75 mmol), prepared and used by the method of Myers et al. (J. Am. Chem. Soc. 1997, 119, 656), and LiCl (1.71 g, 40.5 mmol) in THF (30 mL) was cooled to −78° C. and n-BuLi was added (13.16 mmol, 5.25 mL of a 2.5M solution). After stirring for 20 min at −78° C., the reaction was warmed to 0° C. and stirred an additional 20 minutes. 3-Phenyl-1-bromopropane (1.3 mL, 7.42 mmol) was added and the reaction was stirred for 2 h at 0° C. Aqueous 1N HCl (50 mL) and EtOAc (50 mL) were added, the organic phase was separated and extracted with 1N HCl (50 mL). The aqueous extracts were combined, cooled in an ice bath and slowly basified to pH 14 with 6N NaOH. The product was extracted with CH2Cl2 (4×50 mL) and the combined extracts were dried over MgSO4 and concentrated to give a yellow oil. Purification by flash chromatography (SiO2 gel, 92:4:4, CH2Cl2:MeOH:triethylamine) delivered 400 mg (78%) of the Product of Example 199, Step A: +APcl MS (M+1)+ 341; 1H NMR=400 MHz (CDCl3) δ: 7.38 (m, 10H), 5.26 (m, 1H), 4.15 (m, 1H), 3.86 (m, 1H), 2.36 (s, 3H).

Aufarbeitung

  1. temperaturethe reaction was warmed to 0° C.
  2. stirringstirred an additional 20 minutes
  3. stirringthe reaction was stirred for 2 h at 0° C
  4. customthe organic phase was separated
  5. extractionextracted with 1N HCl (50 mL)
  6. temperaturecooled in an ice bath and slowly basified to pH 14 with 6N NaOH
  7. extractionThe product was extracted with CH2Cl2 (4×50 mL)
  8. dry with materialthe combined extracts were dried over MgSO4
  9. concentrationconcentrated
  10. customto give a yellow oil
  11. customPurification by flash chromatography (SiO2 gel, 92:4:4, CH2Cl2:MeOH:triethylamine)

Quellen und Nachweise

ORD-Eintrag
ord-43cf9ba3cb66406f8aa527eecb7bef2f
Quelldatensatz
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06251902B1

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