StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Phosgene → HCID 57842704, Verbindung

HRID 735593
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 735593
C(Cl)(Cl)=O.[NH2:5][C:6]1[CH:7]=[C:8]([C@@H:12]([NH:19][C:20]([O:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[O:21])[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:9]=[CH:10][CH:11]=1.[C:30]([O-:33])(O)=[O:31].[Na+].[Br:35][C:36]1[CH:41]=[CH:40][C:39]([CH2:42][CH2:43]O)=[C:38]([CH3:45])[CH:37]=1.[N-]=C=O.[H-].[Na+].[Cl-].[NH4+]>C1COCC1.O>[CH2:23]([O:22][C:20]([NH:19][C@H:12]([C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([NH:5][C:30]([O:33][CH2:43][CH2:42][C:39]2[CH:40]=[CH:41][C:36]([Br:35])=[CH:37][C:38]=2[CH3:45])=[O:31])[CH:7]=1)[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:21])[C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 7

HCID 6371PhosgeneHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 105034IsocyanateHCID 516892Sodium BicarbonateHCID 57842670(S)-ethyl 3-(3-aminophenyl)-3-(benzyloxycarbonylamino)propanoateHCID 57842852
2-(4-Bromo-2-methylphenyl)ethanol

Produkt 1

HCID 57842704HCID 57842704, VerbindungAusbeute 57 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Phosgene (3.5 mmol, 1.75 mL, 20% in toluene) was added to a solution of 34C (600 mg, 1.75 mmol) and NaHCO3 (1.47 g, 17.5 mmol) at 0° C. After stirring for 1 h at rt, the solution was filtered and concentrated in vacuo. 30B (375 mg, 1.75 mmol) in THF (20 mL) was added to the crude isocyanate and the solution was cooled to −45° C. NaH (93 mg) was added in one portion and the mixture was warmed to 0° C. and stirred for 2 h at 0° C. and 15 h at ambient temperature. Ammonium chloride (5 mL, saturated) was added and the reaction mixture was diluted with water and extracted with EtOAc. The organics were combined, washed with brine, dried over Na2SO4 and concentrated in vacuo. The crude product was purified by flash chromatography (0% to 50% EtOAc in hexanes) to yield 34D (578 mg, 57%) as a yellow oil. 1H NMR (400 MHz, CDCl3) δ ppm 1.15 (t, J=7.15 Hz, 3 H) 2.32 (s, 3 H) 2.80-2.87 (m, J=6.87, 6.87 Hz, 2 H) 2.93 (t, J=7.15 Hz, 2 H) 4.05 (q, J=7.15 Hz, 2 H) 4.30 (t, J=7.15 Hz, 2 H) 5.02-5.18 (m, 3 H) 6.95-7.09 (m, 2 H) 7.23-7.37 (m, 10 H).

Aufarbeitung

  1. filtrationthe solution was filtered
  2. concentrationconcentrated in vacuo
  3. temperaturethe solution was cooled to −45° C
  4. temperaturethe mixture was warmed to 0° C.
  5. stirringstirred for 2 h at 0° C. and 15 h at ambient temperature
  6. extractionextracted with EtOAc
  7. washwashed with brine
  8. dry with materialdried over Na2SO4
  9. concentrationconcentrated in vacuo
  10. customThe crude product was purified by flash chromatography (0% to 50% EtOAc in hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-ebc648b8ea664c5b92b74633ea085040
Quelldatensatz
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07592331B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion