Hydrochloric Acid → HCID 178448922, Verbindung

HRID 1030062Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1030062
[CH3:1][C:2]1[N:7]=[C:6]([N:8]([CH2:46][CH2:47][CH2:48][CH3:49])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[N:26](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:25]=[N:24][N:23]=3)=[CH:12][CH:11]=2)[C:5]([C:50]([O:52][CH2:53][CH3:54])=[O:51])=[CH:4][N:3]=1.Cl>C(O)C.C(Cl)(Cl)Cl>[CH3:1][C:2]1[N:7]=[C:6]([N:8]([CH2:46][CH2:47][CH2:48][CH3:49])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[NH:26][N:25]=[N:24][N:23]=3)=[CH:12][CH:11]=2)[C:5]([C:50]([O:52][CH2:53][CH3:54])=[O:51])=[CH:4][N:3]=1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 19791910Ethyl 2-methyl-4-{N-butyl-N-[{2'-(N-triphenylmethyltetrazol-5-yl)biphenyl-4-yl}methyl]amino}pyrimidine-5-carboxylate

Produkt 1

HCID 178448922HCID 178448922, VerbindungAusbeute 89,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

The product of example 1B (3.5 g, 4.91 mmoles) was suspended in 50 ml of ethanol. Concentrated hydrochloric acid (2.1 ml) was added and the mixture was stirred for 11/2 hours at room temperature. The solution was concentrated under vacuum and the resulting residue was diluted with water. Potassium acetate was added in portions until the pH was neutral. Ether (5 ml) was added and the mixture was stirred. The sticky solid which formed was dissolved in chloroform. The chloroform solution was dried over sodium sulfate and then concentrated. The resulting residue was crystallized from ether to provide 2.08 g of the desired product. M.p. 164°-166° C. 1H NMR (CDCl3) δ0.85 (t, 3H, J=7 Hz), 1.25 (m, 2H), 1.32 (t, 3H, J=7 Hz), 1.50 (m, 2H), 2.24 (s, 3H), 3.38 (t, 2H, J=7 Hz), 4.30 (q, 2H, J=7 Hz), 4.73 (s, 2H), 7.00 (m, 4H), 7.42 (dd, 1H, J=8 Hz, J=1Hz), 7.50-7.62 (m, 2H), 7.75 (dd, 1H, J=8 Hz, J= 1Hz), 8.02 (s, 1H).

Aufarbeitung

  1. concentrationThe solution was concentrated under vacuum
  2. additionthe resulting residue was diluted with water
  3. additionPotassium acetate was added in portions until the pH
  4. additionEther (5 ml) was added
  5. stirringthe mixture was stirred
  6. customThe sticky solid which formed
  7. dry with materialThe chloroform solution was dried over sodium sulfate
  8. concentrationconcentrated
  9. customThe resulting residue was crystallized from ether

Quellen und Nachweise

ORD-Eintrag
ord-48b4a44f8f4d4d3d96ee98db5477797d
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05104877

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