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

2-Amino-5-chloropyridine → HCID 66705878, Verbindung

HRID 2276373
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2276373
NC1C=CC(Cl)=CN=1.ClC(Cl)(OC(=O)OC(Cl)(Cl)Cl)Cl.[Cl-].C([NH+](CC)CC)C.[Cl:29][C:30]1[CH:31]=[CH:32][C:33]([N:36]=[C:37]=[O:38])=[N:34][CH:35]=1.[NH2:39][C:40]1[CH:45]=[CH:44][C:43]([CH:46]2[CH2:50][CH2:49][N:48]([C:51]([O:53][C:54]([CH3:57])([CH3:56])[CH3:55])=[O:52])[CH2:47]2)=[CH:42][CH:41]=1.C(N(CC)C(C)C)(C)C>ClC(Cl)C.ClCCl.C(N(CC)CC)C>[C:54]([O:53][C:51]([N:48]1[CH2:49][CH2:50][CH:46]([C:43]2[CH:44]=[CH:45][C:40]([NH:39][C:37]([NH:36][C:33]3[CH:32]=[CH:31][C:30]([Cl:29])=[CH:35][N:34]=3)=[O:38])=[CH:41][CH:42]=2)[CH2:47]1)=[O:52])([CH3:57])([CH3:55])[CH3:56]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 6

HCID 661742-Amino-5-chloropyridineHCID 81531DiisopropylethylamineHCID 94429TriphosgeneHCID 12698378Triethylazanium chlorideHCID 205331395-Chloro-2-isocyanatopyridineHCID 57365069Tert-butyl 3-(4-aminophenyl)pyrrolidine-1-carboxylate

Produkt 1

HCID 66705878
HCID 66705878, Verbindung
Ausbeute 38 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6344DichloromethaneLösungsmittelHCID 63651,1-DichloroethaneLösungsmittel2×HCID 8471TriethylamineLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a stirred suspension of 2-amino-5-chloro-pyridine (1.01 g) in dichloroethane (20 ml) was added portionwise triphosgene (831 mg). Triethylamine (2.22 ml) was then added dropwise and the mixture was stirred at 50° C. for 1 h. The mixture was then concentrated in vacuo to afford a beige solid containing a mixture of triethylammonium chloride and 5-chloro-2-isocyanato-pyridine. This solid was then added to a stirred solution of (RS)-tert-butyl 3-(4-aminophenyl)pyrrolidine-1-carboxylate (350 mg, CAS 908334-28-1) and N,N-diisopropylethylamine (0.68 ml) in dichloroethane (6 ml) and the resulting mixture was stirred at 60° C. overnight. The mixture was then diluted with dichloromethane and washed with water. The phases were separated and the organic phase was dried over sodium sulphate and concentrated in vacuo. The residue was purified by column chromatography (SiO2; gradient: heptane/EtOAc) to give (RS)-3-{4-[3-(5-chloro-pyridin-2-yl)-ureido]-phenyl}-pyrrolidine-1-carboxylic acid tert-butyl ester (212 mg, 38%) as an off-white solid. MS (ISP): 419.2 ([{37Cl}M+H]+), 417.2 ([{35Cl}M+H]+).

Aufarbeitung

  1. concentrationThe mixture was then concentrated in vacuo
  2. customto afford a beige solid
  3. additioncontaining
  4. stirringthe resulting mixture was stirred at 60° C. overnight
  5. washwashed with water
  6. customThe phases were separated
  7. dry with materialthe organic phase was dried over sodium sulphate
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by column chromatography (SiO2; gradient: heptane/EtOAc)

Quellen und Nachweise

ORD-Eintrag
ord-e1aa8b0cb4d34d5cb5acc0a7b471a382
Quelldatensatz
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09132136B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion