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Diisopropylethylamine → N-(4-(Trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine

HRID 2219952
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2219952
ClC(OC(Cl)C)=O.C([N:15]1[CH2:24][CH2:23][C:22]2[C:21]([NH:25][C:26]3[CH:31]=[CH:30][C:29]([C:32]([F:35])([F:34])[F:33])=[CH:28][CH:27]=3)=[N:20][C:19]([S:36][CH3:37])=[N:18][C:17]=2[CH2:16]1)C1C=CC=CC=1.C(N(C(C)C)CC)(C)C>ClCCCl>[F:34][C:32]([F:33])([F:35])[C:29]1[CH:30]=[CH:31][C:26]([NH:25][C:21]2[C:22]3[CH2:23][CH2:24][NH:15][CH2:16][C:17]=3[N:18]=[C:19]([S:36][CH3:37])[N:20]=2)=[CH:27][CH:28]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 5213051-Chloroethyl chloroformateHCID 590215717-benzyl-N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine

Produkt 1

HCID 59021576N-(4-(Trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amineAusbeute 67 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 11
1,2-Dichloroethane
Lösungsmittel

Versuchsvorschrift

1-Chloroethyl chloroformate (572 mg, 4 mmol) was added dropwise to the solution of 7-benzyl-N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine (860 mg, 2 mmol) and diisopropylethyl amine (516 mg, 4 mmol) in 1,2-dichloroethane (5 mL, anhydrous) at 0° C. After addition, the reaction mixture was stirred at room temperature for 1 hr. Solvent was removed in vacuo, residue was dissolved in methanol (10 mL) and was stirred at room temperature overnight. Solvent was removed in vacuo, residue was dissolved in ethyl acetate and was washed by sodium bicarbonate's aqueous solution, brine and dried over sodium sulfate. Solvent was removed in vacuo and residue was triturated by diethyl ether to yield the product as a beige solid (454 mg, 67%).

Aufarbeitung

  1. additionAfter addition
  2. customSolvent was removed in vacuo, residue
  3. dissolutionwas dissolved in methanol (10 mL)
  4. stirringwas stirred at room temperature overnight
  5. customSolvent was removed in vacuo, residue
  6. dissolutionwas dissolved in ethyl acetate
  7. washwas washed by sodium bicarbonate'
  8. dry with materialdried over sodium sulfate
  9. customSolvent was removed in vacuo and residue
  10. customwas triturated by diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-32e05e5659314a1f8a59fba9e429b801
Quelldatensatz
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07414131B2

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