Octane → N-(5-Methyl-2-propargyloxyphenylsulfonyl)-N'-(4-chloro-6-methoxypyrimidin-2-yl)-urea

HRID 325802

Reaktionsgleichung

Reaktionsgleichung von HRID 325802
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([O:14][CH2:15][C:16]#[CH:17])=[C:6]([S:8]([N:11]=[C:12]=[O:13])(=[O:10])=[O:9])[CH:7]=1.[NH2:18][C:19]1[N:24]=[C:23]([Cl:25])[CH:22]=[C:21]([O:26][CH3:27])[N:20]=1.CCCCCCCC>O1CCCC1>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([O:14][CH2:15][C:16]#[CH:17])=[C:6]([S:8]([NH:11][C:12]([NH:18][C:19]2[N:24]=[C:23]([Cl:25])[CH:22]=[C:21]([O:26][CH3:27])[N:20]=2)=[O:13])(=[O:10])=[O:9])[CH:7]=1

Komponenten

5

Versuchsvorschrift

A solution of 9.4 g of crude 5-methyl-2-propargyloxyphenylsulfonylisocyanate in 50 ml of absolute tetrahydrofuran is added dropwise at room temperature, within 10 minutes, to a solution of 3.7 g of 2-amino-4-chloro-6-methoxy-pyrimidine and 0.1 g of 1,4-diazadicyclo[2.2.2]octane in 60 ml of absolute tetrahydrofuran, in the course of which the temperature rises slightly. The reaction solution is stirred for 18 hours at room temperature; it is then filtered, and concentrated by evaporation. The residue is crystallised from ethyl acetate to thus obtain 5.8 g of N-(5-methyl-2-propargyloxyphenylsulfonyl)-N'-(4-chloro-6-methoxy-pyrimidin-2-yl)-urea, m.p. 202°-204° C.

Aufarbeitung

  1. filtrationit is then filtered
  2. concentrationconcentrated by evaporation
  3. customThe residue is crystallised from ethyl acetate to thus obtain 5.8 g of N-(5-methyl-2-propargyloxyphenylsulfonyl)-N'-(4-chloro-6-methoxy-pyrimidin-2-yl)-urea, m.p. 202°-204° C.

Quellen und Nachweise

ORD-Eintrag
ord-d1f601befbce40ebb817445180d90ed2
Quelldatensatz
uspto-grants-1984_04
Patentnummer
US04443243

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