Dobutamine Hydrochloride → Dobutamine

HRID 246858

Reaktionsgleichung

Reaktionsgleichung von HRID 246858
[CH3:1][CH:2]([NH:12][CH2:13][CH2:14][C:15]1[CH:16]=[CH:17][C:18]([OH:22])=[C:19]([OH:21])[CH:20]=1)[CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([OH:11])=[CH:9][CH:10]=1.Cl>O>[CH3:1][CH:2]([NH:12][CH2:13][CH2:14][C:15]1[CH:16]=[CH:17][C:18]([OH:22])=[C:19]([OH:21])[CH:20]=1)[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1

Komponenten

3

Edukt 1

HCID 65324Dobutamine Hydrochloride

Produkt 1

HCID 36811DobutamineAusbeute 95,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Seventeen grams of dobutamine hydrochloride were suspended in 500 ml of deaerated water [deaerated by alternatively applying a vacuum (10-100 Torr.) followed by a period of sparging with N2 ]. 150 mg of sodium sulfite were added as a peroxide scavenger. The suspension was stirred under a constant positive N2 pressure. 50 ml of 1N aqueous sodium hydroxide diluted to 120 ml with deaerated water were added in dropwise fashion over a 2.5 hr. period. After the addition was complete, the neutralization mixture was stirred for an additional 2 hours, during which time a white crystalline solid comprising dobutamine free base separated. The supernate was decanted, and the crystalline residue washed thoroughly with 600 ml of deaerated water. The supernate was again decanted. The solid precipitate was then filtered under N2. The filter cake was washed twice with 100 ml portions of water and was then dried at 45° C. under vacuum for 3 hours. 14.5 g of dobutamine free base were thus obtained.

Aufarbeitung

  1. waitfollowed by a period
  2. customof sparging with N2 ]
  3. addition150 mg of sodium sulfite were added as a peroxide scavenger
  4. addition50 ml of 1N aqueous sodium hydroxide diluted to 120 ml with deaerated water
  5. additionwere added in dropwise fashion over a 2.5 hr
  6. additionAfter the addition
  7. stirringthe neutralization mixture was stirred for an additional 2 hours, during which time a white crystalline solid comprising dobutamine free base
  8. customseparated
  9. customThe supernate was decanted
  10. washthe crystalline residue washed thoroughly with 600 ml of deaerated water
  11. customThe supernate was again decanted
  12. filtrationThe solid precipitate was then filtered under N2
  13. washThe filter cake was washed twice with 100 ml portions of water
  14. customwas then dried at 45° C. under vacuum for 3 hours

Quellen und Nachweise

ORD-Eintrag
ord-b70a5ec37cb847e0a1a39d154f0b6c1c
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04704407

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