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4-Methylmorpholine → 1-[4-(2-Carbamoylpyridin-4-yloxy)-2-fluorophenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester

HRID 409932
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 409932
S(Cl)(Cl)=O.[CH2:5]([O:12][C:13]([C:15]1([C:18]([OH:20])=O)[CH2:17][CH2:16]1)=[O:14])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[NH2:21][C:22]1[CH:38]=[CH:37][C:25]([O:26][C:27]2C=CN=C(CC(N)=O)[CH:28]=2)=[CH:24][C:23]=1[F:39].C[N:41]1[CH2:46][CH2:45][O:44][CH2:43][CH2:42]1.C[N:48]1CCCC1=O>O1CCCC1.O>[CH2:5]([O:12][C:13]([C:15]1([C:18](=[O:20])[NH:21][C:22]2[CH:38]=[CH:37][C:25]([O:26][C:27]3[CH:43]=[CH:42][N:41]=[C:46]([C:45](=[O:44])[NH2:48])[CH:28]=3)=[CH:24][C:23]=2[F:39])[CH2:16][CH2:17]1)=[O:14])[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 79724-MethylmorpholineHCID 13387N-methyl-2-pyrrolidone2×HCID 24386Thionyl ChlorideHCID 574708601-((Benzyloxy)carbonyl)cyclopropanecarboxylic acidHCID 1317316354-(4-Amino-3-fluorophenoxy)pyridine-2-carboxyamide

Produkt 1

HCID 24788499
1-[4-(2-Carbamoylpyridin-4-yloxy)-2-fluorophenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Thionyl chloride was added at −20° C. to a solution of 1-(benzyloxycarbonyl)cyclopropanecarboxylic acid (97.98 g) in tetrahydrofuran (200 ml) and N-methylpyrrolidone (200 ml) and stirred for 30 minutes. A solution of 4-(4-amino-3-fluorophenoxy)pyridine-2-carboxyamide (100 g) and N-methylmorpholine (40.91 g) in N-methylpyrrolidone (600 ml) were added to the reaction mixture at the same temperature and stirred for 1 hour at 10° C. Water (100 g) was added to the reaction mixture and stirred for 1 hour at 20° C. After confirming the crystal precipitation, a 1N sodium hydroxide aqueous solution (1 L) was added and further stirred for 19 hours. The precipitated solid was collected by filtration and washed with water (500 g). The obtained solid was dried for 20 hours at 60° C. to give 176.7 g of the title compound.

Aufarbeitung

  1. stirringstirred for 1 hour at 10° C
  2. stirringstirred for 1 hour at 20° C
  3. customthe crystal precipitation
  4. additiona 1N sodium hydroxide aqueous solution (1 L) was added
  5. stirringfurther stirred for 19 hours
  6. filtrationThe precipitated solid was collected by filtration
  7. washwashed with water (500 g)
  8. customThe obtained solid was dried for 20 hours at 60° C.

Quellen und Nachweise

ORD-Eintrag
ord-f5229ec57e0440a398aace9b2b83cb4b
Quelldatensatz
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08759530B2

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