Ammonia → HCID 21876582, Verbindung

HRID 723786Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 723786
[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2(O)[CH2:14][CH2:13][S:12][CH2:11][CH2:10]2)=[C:4]([F:16])[CH:3]=1.Cl.O.N>C(O)(=O)C>[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2[CH2:14][CH2:13][S:12][CH2:11][CH:10]=2)=[C:4]([F:16])[CH:3]=1

Komponenten

6

Edukt 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 962WaterHCID 9964829HCID 9964829, Verbindung

Produkt 1

HCID 21876582HCID 21876582, VerbindungAusbeute 98,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

4-(4-Amino-2,6-difluoro-phenyl)-tetrahydro-thiopyran-4-o1 (16.7 g, 68 mM) was suspended in a mixture of concentrated hydrochloric acid (200 ml), water (50 ml) and acetic acid (200 ml), BHT (50 mg) added, and the whole stirred under nitrogen at 800 for 18 hours. After cooling, the mixture was made basic by cautious addition of concentrated ammonia, and ice-water. The mixture was then extracted with diethyl ether (2×300 ml), the extracts washed with water (100 ml), brine (200 ml) and dried (magnesium sulfate). Evaporation gave the desired product as a cream solid (15.2 g).

Aufarbeitung

  1. additionadded
  2. temperatureAfter cooling
  3. extractionThe mixture was then extracted with diethyl ether (2×300 ml)
  4. washthe extracts washed with water (100 ml), brine (200 ml)
  5. dry with materialdried (magnesium sulfate)
  6. customEvaporation

Quellen und Nachweise

ORD-Eintrag
ord-d567f90fb43f409d8a449f3ba5ba9c2f
Quelldatensatz
uspto-grants-2006_11
Patentnummer
US07141583B2

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