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

HRID 971233
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 971233
ClC(OC(Cl)C)=O.[C:8]([C:12]1[CH:17]=[CH:16][C:15]([NH:18][C:19]2[C:20]3[CH2:30][CH2:29][N:28](CC4C=CC=CC=4)[CH2:27][C:21]=3[N:22]=[C:23]([S:25][CH3:26])[N:24]=2)=[CH:14][CH:13]=1)([CH3:11])([CH3:10])[CH3:9].C(N(C(C)C)CC)(C)C>ClCCCl>[C:8]([C:12]1[CH:17]=[CH:16][C:15]([NH:18][C:19]2[C:20]3[CH2:30][CH2:29][NH:28][CH2:27][C:21]=3[N:22]=[C:23]([S:25][CH3:26])[N:24]=2)=[CH:14][CH:13]=1)([CH3:11])([CH3:9])[CH3:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 5213051-Chloroethyl chloroformateHCID 59021482N-(4-tert-Butylphenyl)-7-benzyl-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine

Produkt 1

HCID 59021569N-(4-tert-Butylphenyl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amineAusbeute 36 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 11
1,2-Dichloroethane
Lösungsmittel

Versuchsvorschrift

1-Chloroethyl chloroformate (732 mg, 5.12 mmol) was added dropwise to a mixture of N-(4-tert-butylphenyl)-7-benzyl-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine (1.07 g, 2.56 mmol) and diisopropylethyl amine (660 mg, 5.12 mmol) in 1,2-dichloroethane (10 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 with saturated aqueous sodium bicarbonate, brine and dried over sodium sulfate. Solvent was removed in vacuo and residue was triturated by diethyl ether to yield the product as a light brown solid (303 mg, 36%).

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 with saturated aqueous sodium bicarbonate, brine
  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-defd53e020da4f23b10dd22b6fe611b4
Quelldatensatz
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07312330B2

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