Water → HCID 15010190, Verbindung

HRID 1651703Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1651703
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:9][CH:10]=[CH:11][C:12]=2[C:13]#[N:14])=[CH:4][CH:3]=1.ClS([N:19]=[C:20]=O)(=O)=O.CN(C)C=O.O>C(COC)OC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[NH:9][C:10]([C:20]#[N:19])=[CH:11][C:12]=2[C:13]#[N:14])=[CH:6][CH:7]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 6228DimethylformamideHCID 70918Chlorosulfonyl isocyanateHCID 146232102-(4-Chlorophenyl)-1H-pyrrole-3-carbonitrile

Produkt 1

HCID 15010190HCID 15010190, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 80711,2-DimethoxyethaneLösungsmittel

Versuchsvorschrift

A sample of 2-p-chlorophenyl-3-cyanopyrrole, prepared by the method of Example 4, (3.0 g, 0.015 mole) is dissolved in 50 mL of dry dimethoxyethane. To this solution is added chlorosulfonyl isocyanate (3.39 g, 0.024 mole). The addition is exothermic and some cooling is necessary. After stirring 3 hours at room temperature, dimethylformamide (6-7 mL) is added and the solution is stirred 4 hours more. The solution is then poured into water precipitating a white solid (3.4 g, 100%). A sample (1.0 g) is purified by dissolving in ethyl acetate and then passing the solution through a 60 mL course filter funnel packed with silica gel. The filtrate is concentrated to yield 0.7 g of a white solid with m.p. 235°-240° C.

Aufarbeitung

  1. additionThe addition
  2. stirringthe solution is stirred 4 hours more
  3. customA sample (1.0 g) is purified
  4. dissolutionby dissolving in ethyl acetate
  5. filtrationfilter funnel
  6. concentrationThe filtrate is concentrated

Quellen und Nachweise

ORD-Eintrag
ord-c6bc034cbf61492282ead410aac28eeb
Quelldatensatz
uspto-grants-1990_05
Patentnummer
US04929634

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