Hydrochloric Acid → HCID 20285546, Verbindung

HRID 127658

Reaktionsgleichung

Reaktionsgleichung von HRID 127658
[NH2:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([S:13](=[O:20])(=[O:19])[NH:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[C:7]2[OH:12].N1C=CC=CC=1.[O:27]1[CH2:32][CH2:31][N:30]([S:33](Cl)(=[O:35])=[O:34])[CH2:29][CH2:28]1.Cl>O>[C:15]([NH:14][S:13]([C:6]1[CH:5]=[CH:4][C:3]2[C:8](=[CH:9][CH:10]=[CH:11][C:2]=2[NH:1][S:33]([N:30]2[CH2:31][CH2:32][O:27][CH2:28][CH2:29]2)(=[O:35])=[O:34])[C:7]=1[OH:12])(=[O:20])=[O:19])([CH3:17])([CH3:16])[CH3:18]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 12798265Morpholine-4-sulfonyl chlorideHCID 204626005-Amino-N-tert-butyl-1-hydroxynaphthalene-2-sulfonamide

Produkt 1

HCID 20285546HCID 20285546, VerbindungAusbeute 72 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a mixture of 9 g. of 5-amino-2-tert-butylsulfamoyl-1-naphthol with 90 ml. of pyridine were added portionwise under ice-cooling and stirring 11 g. of morpholinosulfonyl chloride and stirring was continued at room temperature for 20 hours. Thereafter, 10 ml. of water were added and stirring was carried out for further 1 hour. Into a mixture of 115 ml. of conc. hydrochloric acid with 400 ml. of ice-water was poured the above reaction mixture to separate a solid precipitate, which was then collected on a filter funnel and washed with water. The product was dissolved in an alkaline solution of 6 g. of sodium hydroxide in 150 ml. of water, insolubles were filtered off, the filtrate was poured into a mixture of 15 ml. of conc. hydrochloric acid with 150 ml. of ice-water to separate a solid precipitate. The precipitate was collected on a filter funnel, washed well with water and then dried to afford 9.6 g. of the desired product in a yield of 72%. mp. 105°-110° C.

Aufarbeitung

  1. additionTo a mixture of 9 g
  2. temperaturecooling
  3. stirringstirring
  4. waitwas carried out for further 1 hour
  5. additionInto a mixture of 115 ml
  6. customto separate a solid precipitate, which
  7. customwas then collected on a filter funnel
  8. washwashed with water
  9. dissolutionThe product was dissolved in an alkaline solution of 6 g
  10. filtrationof water, insolubles were filtered off
  11. additionthe filtrate was poured into a mixture of 15 ml
  12. customof ice-water to separate a solid precipitate
  13. customThe precipitate was collected on a filter funnel
  14. washwashed well with water
  15. customdried
  16. customto afford 9.6 g

Quellen und Nachweise

ORD-Eintrag
ord-8c93f19e76ba42cf937a14f08e65a2e2
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04256831

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