Water → HCID 20237825, Verbindung

HRID 365196Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 365196
Cl[C:2]1[N:3]([CH3:12])[C:4](=[O:11])[N:5]([CH3:10])[C:6](=[O:9])[C:7]=1[CH3:8].[O:13]([CH2:20][CH:21]([OH:30])[CH2:22][NH:23][CH2:24][C:25]([CH3:29])([CH3:28])[CH2:26][NH2:27])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.N1C=CC=CC=1.O>C(Cl)Cl>[O:13]([CH2:20][CH:21]([OH:30])[CH2:22][NH:23][CH2:24][C:25]([CH3:28])([CH3:29])[CH2:26][NH:27][C:2]1[N:3]([CH3:12])[C:4](=[O:11])[N:5]([CH3:10])[C:6](=[O:9])[C:7]=1[CH3:8])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 1049PyridineHCID 132969876-Chloro-1,3,5-trimethyl-2,4(1H,3H)-pyrimidinedioneHCID 20237895HCID 20237895, Verbindung

Produkt 1

HCID 20237825HCID 20237825, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

4.5 g. 4-Chloro-1,3,5-trimethylpyrimidine-2,6(1H,3H)-dione and 6.1 g. 1-phenoxy-3-(3-amino-2,2-dimethylpropylamino)-propan-2-ol (b.p. 159°-161° C./0.01 mm.Hg; obtained from phenyl glycidyl ether and 2,2-dimethyl-1,3-diaminopropane) are stirred for 50 hours at 80° C. in 8 ml. pyridine. The reaction mixture is taken up in methylene chloride, shaken with water, dried, evaporated and the residue obtained chromatographed on silica gel in the manner described in Example 29 to give 2.3 g. (24% of theory) of the desired product in the form of colorless crystals; m.p. 111°-112° C., after recrystallization from ethyl acetate.

Aufarbeitung

  1. customdried
  2. customevaporated
  3. customthe residue obtained
  4. customchromatographed on silica gel in the manner
  5. customto give 2.3 g

Quellen und Nachweise

ORD-Eintrag
ord-df68696b9e5246bbb82e13a148c23586
Quelldatensatz
uspto-grants-1986_08
Patentnummer
US04608383

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