Hydrochloric Acid → Ethyl 2,3-dihydro-1H-inden-2-ylcarbamate

HRID 327023

Reaktionsgleichung

Reaktionsgleichung von HRID 327023
C(N(CC)CC)C.Cl.[NH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11]1.Cl[C:20]([O:22][CH2:23][CH3:24])=[O:21].Cl>ClCCl>[CH2:11]1[C:12]2[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:18][CH:10]1[NH:9][C:20]([O:22][CH2:23][CH3:24])=[O:21]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 1227642-Aminoindan hydrochloride

Produkt 1

HCID 15132155Ethyl 2,3-dihydro-1H-inden-2-ylcarbamateAusbeute 70,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

200 ml of dichloromethane then 10 ml, i.e. 7.26 g (71.7 mmol) of triethylamine were added to 5 g (29.5 mmol) of 2-aminoindan hydrochloride. The mixture was stirred for 30 min, then 3.4 ml, i.e. 3.84 g (35.4 mmol) of ethyl chloroformate were added dropwise. The mixture was stirred for 30 min, then ice-water and an excess of 1N hydrochloric acid were added. The precipitate was filtered, washed, dried and purified by chromatography on a silica gel column, eluted with an 80:20 mixture of dichloromethane/ethyl acetate. 4.25 g of amorphous solid were isolated.

Aufarbeitung

  1. stirringThe mixture was stirred for 30 min
  2. filtrationThe precipitate was filtered
  3. washwashed
  4. customdried
  5. custompurified by chromatography on a silica gel column
  6. washeluted with an 80:20 mixture of dichloromethane/ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-928abd9a69274123ae53332b8189f2b0
Quelldatensatz
uspto-grants-1993_12
Patentnummer
US05272157

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