Hydrochloric Acid → HCID 57471403, Verbindung

HRID 1044522Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1044522
[CH2:1]([CH:8]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:18]#[N:19])[CH:16]=2)[CH2:11][CH2:10][CH:9]1[NH:20]C(=O)OC(C)(C)C)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>ClCCl.C(O)(C)C>[NH2:20][CH:9]1[CH:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:17]2[CH:16]=[C:15]([C:18]#[N:19])[CH:14]=[CH:13][C:12]=2[CH2:11][CH2:10]1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 57467306HCID 57467306, Verbindung

Produkt 1

HCID 57471403HCID 57471403, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3776IsopropanolLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Tert-butyl 1-benzyl-7-cyano-1,2,3,4-tetrahydronaphthalen-2-ylcarbamate (1.1 g, 3.03 mmol) was dissolved in dichloromethane (20 mL) and 5 M hydrochloric acid in isopropanol (2 mL) was added. The reaction mixture was stirred at room temperature for 12 h followed by 4 h at 35° C. The solvent was evaporated in vacuo. Water (30 mL) was added and the pH was adjusted to pH 9 using aqueous saturated sodium bicarbonate solution. The aqueous layer was extracted with dichloromethane. The combined extracts were dried (MgSO4) and the solvent was evaporated in vacuo. Yield: 790 mg (3.03 mmol, 100%).

Aufarbeitung

  1. waitfollowed by 4 h at 35° C
  2. customThe solvent was evaporated in vacuo
  3. additionWater (30 mL) was added
  4. extractionThe aqueous layer was extracted with dichloromethane
  5. dry with materialThe combined extracts were dried (MgSO4)
  6. customthe solvent was evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5c7c2d61b51440b9a5d2418ff53e6e6d
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08563617B2

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