Hydrochloric Acid → Ethyl 5,6,7,8-tetrahydro-4H-thieno[2,3-d]azepine-2-carboxylate hydrochloride

HRID 1648933Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1648933
C([N:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[C:16]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[S:17][C:11]=2[CH2:10][CH2:9]1)C1C=CC=CC=1.[ClH:23]>C(O)C.[Pd]=O>[ClH:23].[S:17]1[C:11]2[CH2:10][CH2:9][NH:8][CH2:14][CH2:13][C:12]=2[CH:15]=[C:16]1[C:18]([O:20][CH2:21][CH3:22])=[O:19]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 13072038ethyl 6-benzyl-5,6,7,8-tetrahydro-4H-thieno[2,3-d]azepine-2-carboxylate

Produkt 1

HCID 20481328Ethyl 5,6,7,8-tetrahydro-4H-thieno[2,3-d]azepine-2-carboxylate hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 5083724Palladium monoxideKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

15.4 gm (0.049 mol) of ethyl 6-benzyl-5,6,7,8-tetrahydro-4H-thieno[2,3-d]-azepine-2-carboxylate were dissolved in 200 of ethyl alcohol by the addition of 50 ml of 1 N hydrochloric acid. After the addition of 5 gm of palladium oxide, the mixture was hydrogenated in an autoclave for 3 hours at 80° C. and under a hydrogen pressure of 5 bars. After the reaction mixture had been cooled, the catalyst was filtered off, the filtrate was evaporated, and the residue was triturated with acetone. The product was suction-filtered and washed several times with acetone.

Aufarbeitung

  1. temperatureAfter the reaction mixture had been cooled
  2. filtrationthe catalyst was filtered off
  3. customthe filtrate was evaporated
  4. customthe residue was triturated with acetone
  5. filtrationThe product was suction-filtered
  6. washwashed several times with acetone

Quellen und Nachweise

ORD-Eintrag
ord-4383cb1e7e704faca0488ab4e0b3fa8c
Quelldatensatz
uspto-grants-1983_11
Patentnummer
US04414225

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