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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → Bavisant dihydrochloride anhydrous

HRID 1192763
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1192763
[ClH:1].[N:2]1([CH2:8][C:9]2[CH:17]=[CH:16][C:12]([C:13]([OH:15])=O)=[CH:11][CH:10]=2)[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.O.ON1C2C=CC=CC=2N=N1.[CH:29]1([N:32]2[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]2)[CH2:31][CH2:30]1.Cl.CN(C)CCCN=C=NCC>C(#N)C.C1(C)C=CC=CC=1>[ClH:1].[ClH:1].[CH:29]1([N:32]2[CH2:37][CH2:36][N:35]([C:13]([C:12]3[CH:11]=[CH:10][C:9]([CH2:8][N:2]4[CH2:3][CH2:4][O:5][CH2:6][CH2:7]4)=[CH:17][CH:16]=3)=[O:15])[CH2:34][CH2:33]2)[CH2:31][CH2:30]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27292554-(Morpholin-4-ylmethyl)benzoic acid hydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 47420041-Cyclopropylpiperazine

Produkt 1

HCID 66712477Bavisant dihydrochloride anhydrous

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittel2×HCID 6342AcetonitrileLösungsmittel2×

Reaktionsbedingungen

Temperatur
22.5 °C

Versuchsvorschrift

A 100-L glass-lined reactor was charged with toluene (45.00 kg) and stirred at ˜20-25° C. To the stirring toluene was added 4-(4-morpholinylmethyl)benzoic acid hydrochloride (6.50 kg, 93.5%, 24.04 mol), 1-hydroxybenzotriazole monohydrate (2.32 kg, 15.13 mol), 1-cyclopropylpiperazine (3.50 kg, 27.07 mol) and acetonitrile (9.00 kg). The resulting off-white slurry was stirred under N2 at ˜20-25° C. for 40 minutes. N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (3.50 kg, 27.07 mol) was added, followed by an acetonitrile (1.20 kg) rinse. After the addition, the reaction mixture was stirred at ˜20-25° C. overnight. Water (32.50 kg) and aqueous saturated sodium carbonate (19.50 L) were then added to the stirring suspension. The suspension was stirred for an additional 30 minutes. The resulting biphasic solution was allowed to settle. The aqueous phase was discarded and the organic phase was washed with a 50% brine solution [water (19.50 L)/brine (19.50 L)]. To the stirred organic phase was then added anhydrous sodium sulfate (2.86 kg) and the resulting mixture was stirred at ˜20-25° C. for 1.5 hours. The solid sodium sulfate was filtered off and the filter cake was washed with acetonitrile (15.30 kg). The filtrate was transferred to a clean 100-L glass-lined reactor and stirred at ˜20-25° C. Water (0.47 kg) and 5/6N HCl in 2-propanol were added to precipitate the title compound as the corresponding bis-hydrochloride salt as a solid. The solid was filtered, washed with acetonitrile (10.2 kg) and dried (60 Torr, ˜40-45° C.) to a constant weight to yield the title compound as a white solid.

Aufarbeitung

  1. stirringThe resulting off-white slurry was stirred under N2 at ˜20-25° C. for 40 minutes
  2. washrinse
  3. additionAfter the addition
  4. stirringthe reaction mixture was stirred at ˜20-25° C. overnight
  5. additionWater (32.50 kg) and aqueous saturated sodium carbonate (19.50 L) were then added to the stirring suspension
  6. stirringThe suspension was stirred for an additional 30 minutes
  7. washthe organic phase was washed with a 50% brine solution [water (19.50 L)/brine (19.50 L)]
  8. stirringadded anhydrous sodium sulfate (2.86 kg) and the resulting mixture was stirred at ˜20-25° C. for 1.5 hours
  9. filtrationThe solid sodium sulfate was filtered off
  10. washthe filter cake was washed with acetonitrile (15.30 kg)
  11. stirringstirred at ˜20-25° C
  12. additionWater (0.47 kg) and 5/6N HCl in 2-propanol were added
  13. customto precipitate the title compound as the corresponding bis-hydrochloride salt as a solid
  14. filtrationThe solid was filtered
  15. washwashed with acetonitrile (10.2 kg)
  16. customdried (60 Torr, ˜40-45° C.) to a constant weight

Quellen und Nachweise

ORD-Eintrag
ord-fbe38c60c5834cb5b6354917f0f6c755
Quelldatensatz
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08680273B2

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