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Acetic Acid → 9-chloro-7-(2-chlorophenyl)-6,7-dihydro-2-methyl-5H-pyrimido[5,4-d][2] benzazepine dihydrochloride

HRID 1979566
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1979566
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[C:6]3[N:21]=[C:20]([CH3:22])[N:19]=[CH:18][C:7]=3[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1.C(O)(=O)C>C(Cl)Cl.[Zn]>[ClH:1].[ClH:1].[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[C:6]3[N:21]=[C:20]([CH3:22])[N:19]=[CH:18][C:7]=3[CH2:8][NH:9][CH:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1
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Komponenten

5

Edukt 2

HCID 176Acetic AcidHCID 132255009-chloro-7-(2-chlorophenyl)-2-methyl-5H-pyrimido[5,4-d][2]benzazepine

Produkt 1

HCID 132255279-chloro-7-(2-chlorophenyl)-6,7-dihydro-2-methyl-5H-pyrimido[5,4-d][2] benzazepine dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23994ZincKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 3.7 g (10.5 mmole) of 9-chloro-7-(2-chlorophenyl)-2-methyl-5H-pyrimido[5,4-d][2]benzazepine, 1.3 g of zinc dust, and 40 ml of acetic acid in 90 ml of methylene chloride was stirred at -15° C. to -20° C. for 30 min. The mixture was filtered over hyflo, and the filtrate was basified with cold dilute aqueous sodium hydroxide and extracted with methylene chloride. The methylene chloride solution was dried over anhydrous sodium sulfate and concentrated at reduced pressure to give a yellow oil. The yellow oil was crystallized from an excess of 6% methanolic hydrogen chloride to give the title compound as a white solid, m.p. 272°-274° C. Recrystallization from methanol gave colorless rods, m.p. 272°-274° C.

Aufarbeitung

  1. filtrationThe mixture was filtered over hyflo
  2. extractionextracted with methylene chloride
  3. dry with materialThe methylene chloride solution was dried over anhydrous sodium sulfate
  4. concentrationconcentrated at reduced pressure
  5. customto give a yellow oil
  6. customThe yellow oil was crystallized from an excess of 6% methanolic hydrogen chloride

Quellen und Nachweise

ORD-Eintrag
ord-d26b0cc6076445b3bbfa688db2985668
Quelldatensatz
uspto-grants-1984_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04481142

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