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Ethanol → DW-1350

HRID 732248
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 732248
[CH:1]([C:4]1[S:8][C:7]([CH3:9])=[N:6][C:5]=1[C:10]1[CH:30]=[CH:29][C:13]([O:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][O:20][C:21]2[CH:28]=[CH:27][C:24]([C:25]#[N:26])=[CH:23][CH:22]=2)=[CH:12][CH:11]=1)([CH3:3])[CH3:2].C(O)C.Cl.[NH2:35][OH:36].C(N(CC)CC)C>O>[OH:36][NH:35][C:25](=[NH:26])[C:24]1[CH:23]=[CH:22][C:21]([O:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][O:14][C:13]2[CH:29]=[CH:30][C:10]([C:5]3[N:6]=[C:7]([CH3:9])[S:8][C:4]=3[CH:1]([CH3:2])[CH3:3])=[CH:11][CH:12]=2)=[CH:28][CH:27]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 702EthanolHCID 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 162024464-{5-[4-(5-Isopropyl-2-Methyl-1,3-Thiazol-4-Yl)-Phenoxy]-Pentoxy}-Benzonitrile

Produkt 1

HCID 178432563DW-1350Ausbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962
Water
Lösungsmittel

Versuchsvorschrift

While 45 g of 4-5-[4-(5-isopropyl-2-methyl-1,3-thiazol-4-yl)-phenoxy]-pentoxy-benzonitrile (10) prepared in Example 6 were added to 300 ml of ethanol and stirred, 15 g of hydroxylamine hydrochloride and 30 ml of triethylamine were added. The temperature was gradually increased and stirring under reflux was continued for 15 hr. After the reaction was completed, the temperature was decreased to 40° C., and the resultant reaction solution was slowly added with water, thereby being crystallized. The precipitated solid was filtered and washed with water, thus obtaining 44.2 g (yield: 95%) of a title compound as a white solid.

Aufarbeitung

  1. temperatureThe temperature was gradually increased
  2. stirringstirring
  3. temperatureunder reflux
  4. customwas decreased to 40° C.
  5. customthe resultant reaction solution
  6. custombeing crystallized
  7. filtrationThe precipitated solid was filtered
  8. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-1399806e59e64f8f8ec64ab6507d2a36
Quelldatensatz
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07585979B2

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