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Hydrochloric Acid → HCID 178433880, Verbindung

HRID 1511522
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1511522
[NH2:1][C:2]1[C:3]([OH:17])=[C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([OH:16])=[O:15])[CH:9]=2)[CH:5]=[CH:6][CH:7]=1.Cl.N([O-])=O.[Na+].S(=O)(=O)(O)[NH2:24].[CH3:28][C:29]1[CH:30]=[C:31]([N:36]2[C:40]([OH:41])=[CH:39][C:38]([CH3:42])=[N:37]2)[CH:32]=[CH:33][C:34]=1[CH3:35]>O.C(N(CC)CC)C.CO>[CH3:35][C:34]1[CH:33]=[CH:32][C:31]([N:36]2[N:37]=[C:38]([CH3:42])/[C:39](=[N:24]/[NH:1][C:2]3[CH:7]=[CH:6][CH:5]=[C:4]([C:8]4[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([OH:16])=[O:15])[CH:9]=4)[C:3]=3[OH:17])/[C:40]2=[O:41])=[CH:30][C:29]=1[CH3:28]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 313Hydrochloric Acid2×HCID 5987Sulfamic AcidHCID 114923323-(3-Amino-2-hydroxyphenyl)benzoic acidHCID 23668193Sodium NitriteHCID 178429255HCID 178429255, Verbindung

Produkt 1

HCID 178433880HCID 178433880, Verbindung
Ausbeute 95,4 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel2×HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

3′-Amino-2′-hydroxybiphenyl-3-carboxylic acid (“BPCA”) Form I (90 g, 392.6 mmol), was added slowly with stirring at room temperature to a solvent mixture of tech. methanol (1.8 L) and 4 M hydrochloric acid (0.245 L, 981.5 mmol) in 3 L reactor. The resulting red solution was stirred for thirty minutes. The solution was then cooled to 0-5° C. and a cold solution of sodium nitrite (27 g, 391.3 mmol) in 90 mL of water was added over twenty minutes such that the reaction mixture temperature did not rise above 10° C. The reaction mixture was stirred for one hour at 5-10° C. Sulfamic acid (4 g, 41.2 mmol) in 90 mL of water was added at 5° C. and the resulting mixture was stirred for additionally one hour at the same temperature. The reaction mixture was warmed to room temperature and triethylamine (ca 104 mL) was added to adjust pH 7-8. 1-(3,4-dimethylphenyl)-3-methyl-1H-pyrazol-5-ol (“pyrazole”) form I (72 g, 357.8 mmol), was added in one portion to the reaction mixture and the resulting mixture was stirred for additionally two hours at room temperature. Hydrochloric acid (4M, ca 140 mL) was slowly added with stirring over twenty minutes to adjust pH to 1.8. A solid precipitated and was collected by filtration, washed with of mixture MeOH:water (1:1, 100 mL) and dried at 40° C./0 bar in vacuum oven for about 18 hours giving 151 g of crude orange to brown crystals of Eltrombopag crude (XRPD: form III with small percentage (less than 10%) of form I. (HPLC: 98.5%, Yield=95.4%)

Aufarbeitung

  1. stirringThe resulting red solution was stirred for thirty minutes
  2. temperatureThe solution was then cooled to 0-5° C.
  3. customdid not rise above 10° C
  4. stirringThe reaction mixture was stirred for one hour at 5-10° C
  5. stirringthe resulting mixture was stirred for additionally one hour at the same temperature
  6. temperatureThe reaction mixture was warmed to room temperature
  7. stirringthe resulting mixture was stirred for additionally two hours at room temperature
  8. stirringwith stirring over twenty minutes
  9. customA solid precipitated
  10. filtrationwas collected by filtration
  11. washwashed with of mixture MeOH:water (1:1, 100 mL)
  12. customdried at 40° C./0 bar in vacuum oven for about 18 hours

Quellen und Nachweise

ORD-Eintrag
ord-dd4ccad7bf654862b4700e7532454faf
Quelldatensatz
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08217021B2

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