Water → N,N-dibenzyl-6-chloro-5-nitropyrimidin-4-amine

HRID 1497998Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1497998
[CH2:1]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:16][C:17]1[C:22]([N+:23]([O-:25])=[O:24])=[C:21](Cl)[N:20]=[CH:19][N:18]=1.C(N(CC)CC)C.O>ClCCl>[CH2:9]([N:8]([CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:21]1[C:22]([N+:23]([O-:25])=[O:24])=[C:17]([Cl:16])[N:18]=[CH:19][N:20]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 7656DibenzylamineHCID 8471TriethylamineHCID 203124,6-Dichloro-5-nitropyrimidine

Produkt 1

HCID 23477266N,N-dibenzyl-6-chloro-5-nitropyrimidin-4-amineAusbeute 105 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A solution of dibenzylamine (10.2 g) in dichloromethane (30 mL) was dripped into a solution of 4,6-dichloro-5-nitropyrimidine (10 g) in dichloromethane (70 mL) on an ice bath. Then triethylamine (14.4 mL) was added, and the mixture was stirred for 1 hour. Water was added to the reaction mixture, the organic layer was washed with a saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate, and the solvent was concentrated under reduced pressure to obtain the title compound (19.2 g) with the physical property value shown below.

Aufarbeitung

  1. washthe organic layer was washed with a saturated aqueous sodium chloride solution
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationthe solvent was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-80a5aff0fd7441ccbf318f407ae418f3
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09199997B2

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