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1-Chloroethyl chloroformate → 2-chloro-N-methyl-N-(1-methylethyl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine hydrochloride

HRID 1879769
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1879769
C([N:8]1[CH2:14][C:13]2[N:15]=[C:16]([Cl:24])[C:17]([N:19]([CH3:23])[CH:20]([CH3:22])[CH3:21])=[N:18][C:12]=2[O:11][CH2:10][CH2:9]1)C1C=CC=CC=1.ClC(OC(Cl)C)=O>C1(C)C=CC=CC=1>[ClH:24].[Cl:24][C:16]1[C:17]([N:19]([CH3:23])[CH:20]([CH3:21])[CH3:22])=[N:18][C:12]2[O:11][CH2:10][CH2:9][NH:8][CH2:14][C:13]=2[N:15]=1
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Komponenten

4

Edukt 2

HCID 5213051-Chloroethyl chloroformateHCID 866490038-benzyl-2-chloro-N-methyl-N-(1-methylethyl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine

Produkt 1

HCID 866490132-chloro-N-methyl-N-(1-methylethyl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine hydrochlorideAusbeute 120,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of 8-benzyl-2-chloro-N-methyl-N-(1-methylethyl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine (200 mg) in toluene (3 mL) was added 1-chloroethyl chloroformate (0.075 mL), and the mixture was stirred at 80° C. for 2 hr. The reaction mixture was cooled to room temperature, and concentrated. To the obtained residue was added methanol (3 ml) and the mixture was stirred at 80° C. for 1 hr. The reaction mixture was cooled to room temperature, and concentrated. The obtained residue was purified by recrystallization (methanol-diisopropyl ether) to give the title compound (102 mg, 60%) as pale-yellow crystals.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationconcentrated
  3. additionTo the obtained residue was added methanol (3 ml)
  4. stirringthe mixture was stirred at 80° C. for 1 hr
  5. temperatureThe reaction mixture was cooled to room temperature
  6. concentrationconcentrated
  7. customThe obtained residue was purified by recrystallization (methanol-diisopropyl ether)

Quellen und Nachweise

ORD-Eintrag
ord-df928cc7bc284006a22ca96383a9886e
Quelldatensatz
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08318722B2

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