Hydrochloric Acid → HCID 12274208, Verbindung

HRID 1579378Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1579378
[ClH:1].[N:2]1[CH:7]=[CH:6][CH:5]=[C:4]2[CH2:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[O:11][C:3]=12.[CH2:16]=O.S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:1][CH2:16][C:14]1[CH:13]=[CH:12][C:10]2[O:11][C:3]3=[N:2][CH:7]=[CH:6][CH:5]=[C:4]3[CH2:8][C:9]=2[CH:15]=1

Komponenten

7

Edukt 5

HCID 313Hydrochloric Acid2×HCID 712Formaldehyde2×HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 122742075H-chromeno[2,3-b]pyridine

Produkt 1

HCID 12274208HCID 12274208, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Hydrogen chloride gas is passed through a mixture of 10 g of 5H-[1]benzopyrano[2,3-b]pyridine, 1.4 g of paraformaldehyde, 110 ml of concentrated sulfuric acid and 22 ml of concentrated hydrochloric acid at 80°C for 12 hours, while 2 g of paraformaldehyde is added in several portions to the reaction mixture. The reaction mixture is poured into water, and the whole mixture is neutralized with sodium carbonate, and extracted with a large amount of chloroform. The chloroform layer is dried, concentrated to 30 ml, and cooled. The crystalline precipitate is filtered off, and recrystallized from chloroform to give 7-chloromethyl-5H-[1]benzopyrano[2,3-b]pyridine melting at 172°-174°C.

Aufarbeitung

  1. additionis added in several portions to the reaction mixture
  2. extractionextracted with a large amount of chloroform
  3. dry with materialThe chloroform layer is dried
  4. concentrationconcentrated to 30 ml
  5. temperaturecooled
  6. filtrationThe crystalline precipitate is filtered off
  7. customrecrystallized from chloroform

Quellen und Nachweise

ORD-Eintrag
ord-e603d10ad4084d83a811f6875b59cedb
Quelldatensatz
uspto-grants-1976_01
Patentnummer
US03931199

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