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

tert-Butyl bromoacetate → Benzyl 4-(2-oxo-1,3-diazinan-1-yl)piperidine-1-carboxylate

HRID 1278985
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1278985
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH:14]([N:17]2[CH2:22][CH2:21][CH2:20][N:19](CC(O)=O)[C:18]2=[O:27])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(C)([O-])C.[K+].BrCC(OC(C)(C)C)=O>O1CCCC1.ClCCl.[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH2:1]([O:8][C:9]([N:11]1[CH2:12][CH2:13][CH:14]([N:17]2[CH2:22][CH2:21][CH2:20][NH:19][C:18]2=[O:27])[CH2:15][CH2:16]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 3

HCID 79177tert-Butyl bromoacetate2×HCID 22137504[3-{1-[(Benzyloxy)carbonyl]piperidin-4-yl}-2-oxotetrahydropyrimidin-1(2H)-yl]acetic acidHCID 23665647Potassium tert-butoxide2×

Produkt 1

HCID 22137530Benzyl 4-(2-oxo-1,3-diazinan-1-yl)piperidine-1-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 67553
Tetrabutylammonium Iodide
Katalysator
HCID 6344DichloromethaneLösungsmittel2×
HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

1-Benzyloxycarbonyl-4-(3-carboxymethyl-2-oxoperhydropyrimidin-1-yl)piperidine. Potassium tert-butoxide (52 mL, 1 M in tert-butanol) was added to l-benzyloxycarbonyl-4-(2-oxoperhydropyrimidin-1-yl)piperidine (15.0 g), and the solution was stirred for 35 minutes. tert-Butyl bromoacetate (7.65 mL) was then added, and the mixture was stirred overnight. The reaction mixture was diluted with tetrahydrofuran (20 mL) and dichloromethane (10 mL) followed by the addition of tetrabutylammonium iodide (1.74 g), potassium tert-butoxide (52 mL, 1 M in tert-butanol), and tert-butyl bromoacetate (7.65 mL). After being stirred overnight, the reaction mixture was diluted with dichloromethane and washed with water. The separated organic layer was dried, evaporated to an oil, and dissolved in 1 N hydrochloric acid (700 mL), tetrahydrofuran (200 mL), and methanol (200 mL). After being stirred overnight, the reaction mixture was concentrated in vacuo to remove the organic solvents. The resulting aqueous solution was extracted with dichloromethane, acidified with 2 N hydrochloric acid to a pH of 2, and extracted with dichloromethane. The first organic extract was concentrated to give unreacted 1-benzyloxycarbonyl-4-(2-oxoperhydropyrimidin-1-yl)piperidine (7.0 g). The second organic extract was washed with water, dried, and evaporated. The crude product was triturated from ether and filtered to give the title compound as a white solid (8.3 g); MS: m/z=376(M+1); NMR (CDCl3): 7.35 (m,5), 5.12 (s,2), 4.48 (m,1), 4.28 (m,2), 4.02 (s,2), 3.35 (m,2), 3.18 (m,2), 2.87 (m,2), 1.97 (m,2), 1.65 (m,4).

Aufarbeitung

  1. stirringthe mixture was stirred overnight
  2. stirringAfter being stirred overnight
  3. washwashed with water
  4. customThe separated organic layer was dried
  5. customevaporated to an oil
  6. dissolutiondissolved in 1 N hydrochloric acid (700 mL)
  7. stirringAfter being stirred overnight
  8. concentrationthe reaction mixture was concentrated in vacuo
  9. customto remove the organic solvents
  10. extractionThe resulting aqueous solution was extracted with dichloromethane
  11. extractionextracted with dichloromethane
  12. extractionThe first organic extract
  13. concentrationwas concentrated

Quellen und Nachweise

ORD-Eintrag
ord-beeb88cae8ed471ea3d3070d044a5d3d
Quelldatensatz
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06444809B1

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion