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Water → HCID 13564978, Verbindung

HRID 236574
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 236574
[CH3:1][C:2]1[NH:3][C:4]([CH3:24])=[C:5]([C:18]([O:20][CH2:21][CH2:22][OH:23])=[O:19])[CH:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])[C:7]=1[N+:8]([O-:10])=[O:9].[OH2:25].N1[CH:31]=[CH:30]C=CC=1>C(OC(=O)C)(=O)C>[CH3:1][C:2]1[NH:3][C:4]([CH3:24])=[C:5]([C:18]([O:20][CH2:21][CH2:22][O:23][C:30](=[O:25])[CH3:31])=[O:19])[CH:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])[C:7]=1[N+:8]([O-:10])=[O:9]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 962WaterHCID 1049PyridineHCID 13564994beta-Hydroxyethyl 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-carboxylate

Produkt 1

HCID 13564978HCID 13564978, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7918Acetic AnhydrideLösungsmittel

Versuchsvorschrift

1 g of β-hydroxyethyl 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-carboxylate is stirred overnight in a mixture of 15 ml of pyridine and 15 ml of acetic anhydride. The mixture is poured into water and extracted with ethyl acetate and the extract is washed with 1 N HCl, water, sodium bicarbonate solution and water again, dried and concentrated. The evaporation residue is crystallized with ethanol, filtered off with suction and washed with ethanol. 800 mg of a yellow-coloured compound of melting point 166° C. which is identical to the compound from Preparation Example 1, process variant A are obtained.

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washthe extract is washed with 1 N HCl, water, sodium bicarbonate solution and water again
  3. customdried
  4. concentrationconcentrated
  5. customThe evaporation residue is crystallized with ethanol
  6. filtrationfiltered off with suction
  7. washwashed with ethanol
  8. custom800 mg of a yellow-coloured compound of melting point 166° C. which is identical to the compound from Preparation Example 1, process variant
  9. customA are obtained

Quellen und Nachweise

ORD-Eintrag
ord-df9ca2833d9c4455885a22cbcdb68161
Quelldatensatz
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04645775

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