Sodium Carbonate → HCID 20299671, Verbindung

HRID 1733462Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1733462
[Cl:1][C:2]1[C:11]([Cl:12])=[C:10]2[C:5]([CH2:6][CH2:7][NH:8][CH2:9]2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].Br[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]Br>C(O)C>[ClH:1].[ClH:1].[CH2:20]([N:8]1[CH2:7][CH2:6][C:5]2[C:10](=[C:11]([Cl:12])[C:2]([Cl:1])=[CH:3][CH:4]=2)[CH2:9]1)[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][N:8]1[CH2:7][CH2:6][C:5]2[C:10](=[C:11]([Cl:12])[C:2]([Cl:1])=[CH:3][CH:4]=2)[CH2:9]1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 123681,6-DibromohexaneHCID 123920Isoquinoline, 7,8-dichloro-1,2,3,4-tetrahydro-

Produkt 1

HCID 20299671HCID 20299671, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A suspension of 2.38 g. (10 mmol) of 7,8-dichloro-1,2,3,4-tetrahydroisoquinoline and 3.18 g. (30 mmol) of sodium carbonate in 50 ml. of absolute ethanol were refluxed for 5 minutes. To this suspension was added 1.22 g. (5 mmol) of 1,6-dibromohexane and the mixture refluxed overnight. The reaction was cooled and after standing for 36 hours was filtered of solid precipitate. The resulting solid was suspended in 100 ml. of ethyl acetate and treated with 1 g. of magnesium sulfate. The mixture was filtered and the filtrate treated with 10 ml. of ethereal hydrochloric acid. The resulting precipitate was removed by filtration, washed with ether and dried to give 2,2'-hexylene-bis(7,8-dichloro-1,2,3,4-tetrahydroisoquinoline)dihydrochloride having a melting point of 308°-311° C.

Aufarbeitung

  1. additionA suspension of 2.38 g
  2. additionTo this suspension was added 1.22 g
  3. temperatureThe reaction was cooled
  4. filtrationwas filtered of solid precipitate
  5. additionof ethyl acetate and treated with 1 g
  6. filtrationThe mixture was filtered
  7. additionthe filtrate treated with 10 ml
  8. customThe resulting precipitate was removed by filtration
  9. washwashed with ether
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-926a19c7b4f043448855d4e8ec151208
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04242346

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