Hydrochloric Acid → Propyrisulfuron

HRID 1160780Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1160780
[Cl:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][CH3:12])=[N:6][N:5]2[C:13]=1[S:14]([NH2:17])(=[O:16])=[O:15].[CH3:18][O:19][C:20]1[CH:25]=[C:24]([O:26][CH3:27])[N:23]=[C:22]([NH:28][C:29](=O)[O:30]C2C=CC=CC=2)[N:21]=1.C1CCN2C(=NCCC2)CC1.Cl>O.C(#N)C>[Cl:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][CH3:12])=[N:6][N:5]2[C:13]=1[S:14]([NH:17][C:29]([NH:28][C:22]1[N:21]=[C:20]([O:19][CH3:18])[CH:25]=[C:24]([O:26][CH3:27])[N:23]=1)=[O:30])(=[O:15])=[O:16]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 10945667Carbamic acid, N-(4,6-dimethoxy-2-pyrimidinyl)-, phenyl esterHCID 230281102-Chloro-6-propylimidazo[1,2-b]pyridazine-3-sulfonamide

Produkt 1

HCID 11990852Propyrisulfuron

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

2-Chloro-6-n-propylimidazo[1,2-b]pyridazin-3-ylsulfonamide (0.49 g, 1.78 mmol), phenyl N-(4,6-dimethoxypyrimidin-2-yl)carbamate (0.55 g, 2 mmol) and acetonitrile (5 ml) were introduced into a 25-ml eggplant type flask and stirred at room temperature, and DBU (0.31 g, 2 mmol) was added all at once thereto, and the mixture was stirred at room temperature for 3 hours. After the reaction was completed, the reaction solution was poured into water (50 ml) and adjusted to about pH 2 with dilute hydrochloric acid, whereby crystals were formed. The crystals were collected by filtration, washed with water, acetone and ether in this order and dried under reduced pressure to give the title compound as pale brown crystals.

Aufarbeitung

  1. stirringwas stirred at room temperature for 3 hours
  2. customwhereby crystals were formed
  3. filtrationThe crystals were collected by filtration
  4. washwashed with water, acetone and ether in this order
  5. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-55d19530f34842f4870a0d301a7a7d53
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07816526B2

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