Hydrochloric Acid → HCID 16747649, Verbindung

HRID 1928374

Reaktionsgleichung

Reaktionsgleichung von HRID 1928374
CC(C)(C)C[O:4][S:5]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([C:14]2[N:19]=[C:18]([C:20]3[CH:25]=[C:24]([C:26]4[CH:31]=[CH:30][C:29]([C:32]([F:35])([F:34])[F:33])=[CH:28][CH:27]=4)[CH:23]=[C:22]([CH3:36])[N:21]=3)[CH:17]=[CH:16][CH:15]=2)[CH:9]=1)(=[O:7])=[O:6].C([O-])CC.[Na+].C(N(CC)CCS)C.Cl>C(O)CC.O>[CH3:36][C:22]1[N:21]=[C:20]([C:18]2[CH:17]=[CH:16][CH:15]=[C:14]([C:10]3[CH:9]=[C:8]([S:5]([OH:7])(=[O:4])=[O:6])[CH:13]=[CH:12][CH:11]=3)[N:19]=2)[CH:25]=[C:24]([C:26]2[CH:31]=[CH:30][C:29]([C:32]([F:35])([F:33])[F:34])=[CH:28][CH:27]=2)[CH:23]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 160322-(Diethylamino)ethanethiolHCID 236693631-Propanol, sodium salt (1:1)HCID 866154673-[6'-Methyl-4'-(4-trifluoromethyl-phenyl)-[2,2']bipyridinyl-6-yl]-benzenesulfonic acid 2,2-dimethyl-propyl ester

Produkt 1

HCID 16747649HCID 16747649, VerbindungAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 10311-PropanolLösungsmittel

Versuchsvorschrift

The title compound was prepared from the above described 3-[6′-methyl-4′-(4-trifluoromethyl-phenyl)-[2,2′]bipyridinyl-6-yl]-benzenesulfonic acid 2,2-dimethyl-propyl ester (7.7 g, 14.24 mmol) by refluxing in 1-propanol (15 mL) with sodium propanolate (1.7 M in n-propanol, 20.95 ml, 35.6 mmol) and 2-(diethylamino)ethanthiol (2.48 mL, 16.38 mmol) for 18 h. Cooled to rt, added water (300 mL), added 1 N HCl (ca. 50 mL) until pH 3-4 was reached, stirred for 10 min, filtered the solid off, washed thrice with water, and then with acetone and dried in HV to give the title compound (5.4 g, 81%) as an off-white solid. MS (ISN) 469.1 [(M−H)−].

Aufarbeitung

  1. customThe title compound was prepared from the
  2. filtrationfiltered the solid off,
  3. washwashed thrice with water
  4. dry with materialwith acetone and dried in HV

Quellen und Nachweise

ORD-Eintrag
ord-67c53f26fef24286a54bf2b971a17083
Quelldatensatz
uspto-grants-2012_05
Patentnummer
US08183262B2

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