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ethyl 4-methylene-7,8-dihydro-4H-thieno[2,3-d]azepine-6(5H)-carboxylate → 4-Methyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester

HRID 446716
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 446716
[CH2:1]=[C:2]1[CH2:8][N:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:6][CH2:5][C:4]2[S:14][CH:15]=[CH:16][C:3]1=2>C(O)C>[CH3:1][CH:2]1[C:3]2[CH:16]=[CH:15][S:14][C:4]=2[CH2:5][CH2:6][N:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:8]1
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Komponenten

3

Edukt 1

HCID 58293774ethyl 4-methylene-7,8-dihydro-4H-thieno[2,3-d]azepine-6(5H)-carboxylate

Produkt 1

HCID 593025564-Methyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Compound 1030 (310 mg, 1.31 mmol) was dissolved in ethanol (50 mL). The solution was degassed three times before addition of 10% Pd/C (100 mg). The flask was charged with hydrogen at atmospheric pressure (H2 balloon) and stirred at RT for 14 hours. The catalyst was removed by filtration through diatomaceous earth and the volatiles removed under reduced pressure to yield ethyl 4,5,7,8-tetrahydro-4-methylthieno[3,2-d]azepine-6-carboxylate (Compound 1031), which was used in subsequent reactions without further purification.

Aufarbeitung

  1. customThe solution was degassed three times
  2. additionbefore addition of 10% Pd/C (100 mg)
  3. additionThe flask was charged with hydrogen at atmospheric pressure (H2 balloon)
  4. customThe catalyst was removed by filtration through diatomaceous earth
  5. customthe volatiles removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-90d4f64eb0954a16a562fc473a1adc14
Quelldatensatz
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08481524B2

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