Hydrochloric Acid → HCID 16747649, Verbindung

HRID 1989654

Reaktionsgleichung

Reaktionsgleichung von HRID 1989654
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

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-69f84a9b2e6a48a78cdd9c93c793f288
Quelldatensatz
uspto-grants-2010_01
Patentnummer
US07642264B2

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