Sodium hydride → HCID 67693623, Verbindung

HRID 1417307

Reaktionsgleichung

Reaktionsgleichung von HRID 1417307
[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.[H-].[Na+].[Na].Cl[CH2:17]/[CH:18]=[CH:19]/[CH2:20][N:21]1[C:29](=[O:30])[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:22]1=[O:31]>CN(C)C=O>[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([O:12][CH2:17]/[CH:18]=[CH:19]/[CH2:20][N:21]3[C:29](=[O:30])[C:28]4[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=4)[C:22]3=[O:31])=[CH:8][CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1

Komponenten

6

Edukt 4

HCID 24758Sodium hydrideHCID 823151-(p-Hydroxyphenyl)imidazoleHCID 5360545SodiumHCID 57093742-((2E)-4-chlorobut-2-en-1-yl)-2,3-dihydro-1H-isoindole-1,3-dione

Produkt 1

HCID 67693623HCID 67693623, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 16.0 g of 4-(1H-imidazol-1-yl)phenol in 250 ml of dimethylformamide, is treated with 4.2 g of 60% NaH. To the suspension of the sodium salt, 23.5 g of (E)-2-[4-chloro-2-buten-1-yl)-1H-isoindole-1,3(2H)-dione is added, and the reaction mixture stirred and heated on the steam bath for 16 hours. The dimethylformamide is removed in vacuo, and the residue stirred with 250 ml of water. The insolubles are collected, washed with water, and dried. Recrystallization from ethanol gives the desired product as a solid, m.p. 170°-171° C.

Aufarbeitung

  1. additionis added
  2. temperatureheated on the steam bath for 16 hours
  3. customThe dimethylformamide is removed in vacuo
  4. stirringthe residue stirred with 250 ml of water
  5. customThe insolubles are collected
  6. washwashed with water
  7. customdried
  8. customRecrystallization from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-7e2c0457e8cc4b2d85de1791618a8f7c
Quelldatensatz
uspto-grants-1999_03
Patentnummer
US05877196

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