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Diisopropylethylamine → HCID 23550119, Verbindung

HRID 1814703
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1814703
C(OC(=O)CCNC(=O)C1C=CC(CN)=CC=1)C.C1C2(CCCCC2)CCC(=O)C1.[CH2:31]([O:33][C:34](=[O:59])[CH2:35][CH2:36][NH:37][C:38](=[O:58])[C:39]1[CH:44]=[CH:43][C:42]([CH2:45][NH:46][CH:47]2[CH2:52][CH2:51][C:50]3([CH2:57][CH2:56][CH2:55][CH2:54][CH2:53]3)[CH2:49][CH2:48]2)=[CH:41][CH:40]=1)[CH3:32].C(N(C(C)C)CC)(C)C.[F:69][C:70]1[CH:71]=[C:72]([CH:76]=[C:77]([C:79]([F:82])([F:81])[F:80])[CH:78]=1)[C:73](Cl)=[O:74]>C(#N)C>[CH2:31]([O:33][C:34](=[O:59])[CH2:35][CH2:36][NH:37][C:38](=[O:58])[C:39]1[CH:44]=[CH:43][C:42]([CH2:45][NH:46][CH:47]2[CH2:52][CH2:51][C:50]3([CH2:53][CH2:54][CH2:55][CH2:56][CH2:57]3)[CH2:49][CH2:48]2)=[CH:41][CH:40]=1)[CH3:32].[CH2:31]([O:33][C:34](=[O:59])[CH2:35][CH2:36][NH:37][C:38](=[O:58])[C:39]1[CH:44]=[CH:43][C:42]([CH2:45][N:46]([C:73](=[O:74])[C:72]2[CH:76]=[C:77]([C:79]([F:80])([F:81])[F:82])[CH:78]=[C:70]([F:69])[CH:71]=2)[CH:47]2[CH2:52][CH2:51][C:50]3([CH2:53][CH2:54][CH2:55][CH2:56][CH2:57]3)[CH2:49][CH2:48]2)=[CH:41][CH:40]=1)[CH3:32]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 81531DiisopropylethylamineHCID 5193643-Fluoro-5-(trifluoromethyl)benzoyl chlorideHCID 574172Spiro[5.5]undecan-3-oneHCID 22502126HCID 22502126, VerbindungHCID 23550130HCID 23550130, Verbindung

Produkt 2

HCID 23550119
HCID 23550119, Verbindung
Ausbeute 200,2 %
HCID 23550130HCID 23550130, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Versuchsvorschrift

3-[4-(Spiro[5.5]undec-3-ylaminomethyl)benzoylamino]propionic acid ethyl ester was prepared by reductive alkylation of 3-(4-aminomethyl-benzoylamino)propionic acid ethyl ester with spiro[5.5]undecan-3-one. 3-[4-(Spiro[5.5]undec-3-ylaminomethyl)benzoylamino]propionic acid ethyl ester (200 mg, 499 μmol) was dissolved in acetonitrile (5 mL) and diisopropylethylamine (170 μL) and cooled on an ice bath. Commercially available 3-fluoro-5-(trifluoromethyl)benzoylchloride (136 mg, 602 μmol) dissolved in acetonitrile (5 mL) was added dropwise. The reaction was complete within one hour as shown by HPLC. The solvent was evaporated and water (10 mL) was added to the residue followed by saturated sodium bicarbonate (10 mL). The product was extracted using ethyl acetate (2×50 mL). The combined ethyl acetate extracts were washed with water (20 mL) and brine (20 mL). Drying the organic phases over MgSO4 and evaporation of the solvent afforded 3-(4-{[(3-fluoro-5-trifluoromethylbenzoyl)spiro[5.5]undec-3-yl-amino]methyl}benzoylamino)propionic acid ethyl ester (295 mg) which was hydrolyzed using sodium hydroxide to afford the title compound.

Aufarbeitung

  1. additionwas added dropwise
  2. customThe solvent was evaporated
  3. additionwater (10 mL) was added to the residue
  4. extractionThe product was extracted
  5. washThe combined ethyl acetate extracts were washed with water (20 mL) and brine (20 mL)
  6. customDrying the organic phases
  7. customover MgSO4 and evaporation of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-351041bc342047979ad8ef5cf357ab37
Quelldatensatz
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06875760B2

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