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Potassium Iodide → (6-((Methylsulfonyl)oxy)-2-(4-((methylsulfonyl)oxy)phenyl)benzo(b)thien-3-yl)(4-(2-(1-piperidinyl)ethoxy)phenyl)-, hydrochloride

HRID 1649607
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1649607
[CH3:1][S:2]([O:5][C:6]1[CH:7]=[CH:8][C:9]2[C:13]([C:14](=[O:25])[C:15]3[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][Cl:24])=[CH:17][CH:16]=3)=[C:12]([C:26]3[CH:31]=[CH:30][C:29]([O:32][S:33]([CH3:36])(=[O:35])=[O:34])=[CH:28][CH:27]=3)[S:11][C:10]=2[CH:37]=1)(=[O:4])=[O:3].[NH:38]1[CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]1.[I-].[K+]>CN(C)C=O>[ClH:24].[CH3:1][S:2]([O:5][C:6]1[CH:7]=[CH:8][C:9]2[C:13]([C:14](=[O:25])[C:15]3[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][N:38]4[CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]4)=[CH:17][CH:16]=3)=[C:12]([C:26]3[CH:31]=[CH:30][C:29]([O:32][S:33]([CH3:36])(=[O:35])=[O:34])=[CH:28][CH:27]=3)[S:11][C:10]=2[CH:37]=1)(=[O:4])=[O:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 4875Potassium IodideHCID 8082PiperidineHCID 204789706-Methanesulfonyloxy-2-(4-methanesulfonyloxyphenyl)-3-[4-(2-chloroethoxy)benzoyl]benzo[b]thiophene

Produkt 1

HCID 19603580(6-((Methylsulfonyl)oxy)-2-(4-((methylsulfonyl)oxy)phenyl)benzo(b)thien-3-yl)(4-(2-(1-piperidinyl)ethoxy)phenyl)-, hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228
Dimethylformamide
Lösungsmittel

Versuchsvorschrift

An 0.58 g. portion of 6-methanesulfonyloxy-2-(4-methanesulfonyloxyphenyl)-3-[4-(2-chloroethoxy)-benzoyl]benzo[b]thiophene was combined with 20 ml. of dimethylformamide, 4.8 ml. of piperidine and 100 mg. of potassium iodide, and the mixture was stirred overnight at 40° C. and then at 50° C. for two hours. The mixture was evaporated to a brown oil under vacuum, and the oil was worked up by pouring it into 50 ml. of saturated aqueous sodium bicarbonate and extracting the mixture twice with 40 ml. portions of ethyl acetate. The organic layers were combined, washed twice with 100 ml. portions of saturated aqueous sodium chloride and concentrated under vacuum to an oil. To the oily residue was added 50 ml. of 3% hydrogen chloride in methanol, and the acidic mixture was concentrated again to an oil, which was dissolved in hot denatured ethanol and crystallized. The first crop of purified crystals amounted to 0.4 g. and had a melting point and infrared and ultraviolet spectra identical to those of the products of Preparations 8 and 11.

Aufarbeitung

  1. customThe mixture was evaporated to a brown oil under vacuum
  2. additionby pouring it into 50 ml
  3. extractionof saturated aqueous sodium bicarbonate and extracting the mixture twice with 40 ml
  4. washwashed twice with 100 ml
  5. concentrationportions of saturated aqueous sodium chloride and concentrated under vacuum to an oil
  6. additionTo the oily residue was added 50 ml
  7. concentrationof 3% hydrogen chloride in methanol, and the acidic mixture was concentrated again to an oil, which
  8. dissolutionwas dissolved in hot denatured ethanol
  9. customcrystallized

Quellen und Nachweise

ORD-Eintrag
ord-d05128123e19410a8296b99edaccf687
Quelldatensatz
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04418068

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