Diisopropylethylamine → HCID 178425016, Verbindung

HRID 1480462Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1480462
[NH:1]1[CH:5]=[C:4]([CH2:6][CH2:7][CH2:8][C:9](Cl)=[O:10])[N:3]=[N:2]1.[NH2:12][CH:13]1[CH2:18][CH2:17][N:16]([C:19]([O:21][CH2:22][C:23]2[CH:28]=[C:27]([CH3:29])[CH:26]=[C:25]([CH3:30])[CH:24]=2)=[O:20])[CH2:15][CH2:14]1.CCN(C(C)C)C(C)C>C(Cl)Cl>[NH:1]1[CH:5]=[C:4]([CH2:6][CH2:7][CH2:8][C:9]([NH:12][CH:13]2[CH2:14][CH2:15][N:16]([C:19]([O:21][CH2:22][C:23]3[CH:24]=[C:25]([CH3:30])[CH:26]=[C:27]([CH3:29])[CH:28]=3)=[O:20])[CH2:17][CH2:18]2)=[O:10])[N:3]=[N:2]1

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 867226873,5-Dimethylbenzyl 4-aminopiperidine-1-carboxylateHCID 178521140HCID 178521140, Verbindung

Produkt 1

HCID 178425016HCID 178425016, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a stirred solution of 4-(1H-1,2,3-triazol-4-yl)butanoic acid chloride in DCM (5 ml) at RT (168 mg, 0.967 mmol) was added 3,5-dimethylbenzyl 4-aminopiperidine-1-carboxylate (318 mg, 1.064 mmol) and Huenig's Base (0.338 mL, 1.934 mmol) and the reaction mixture was allowed to stir for 3 hrs. The reaction mixture was diluted with DCM and washed with a saturated solution of brine. The layers were separated and the organic portion dried over MgSO4, filtered and concentrated under reduced pressure. Purification was carried out by chromatography on silica using 0-10% MeOH in DCM as eluent to afford the title product;

Aufarbeitung

  1. washwashed with a saturated solution of brine
  2. customThe layers were separated
  3. dry with materialthe organic portion dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customPurification

Quellen und Nachweise

ORD-Eintrag
ord-b367eeb438974882ac037c6278518740
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09409895B2

Notizen zur Reaktion

Wird geladen…