Water → 5-(4-isopropyl-2-morpholinylmethyl)-10,11-dihydro-5H-dibenz[b,f]azepine

HRID 328581

Reaktionsgleichung

Reaktionsgleichung von HRID 328581
[NH2-].[Na+].[CH:3]1[C:13]2[CH2:12][CH2:11][C:10]3[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=3[NH:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.[CH:18]([N:21]1[CH2:26][CH2:25][O:24][CH:23]([CH2:27]Cl)[CH2:22]1)([CH3:20])[CH3:19].O>C1C=CC=CC=1>[CH:18]([N:21]1[CH2:26][CH2:25][O:24][CH:23]([CH2:27][N:8]2[C:9]3[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=3[CH2:11][CH2:12][C:13]3[CH:3]=[CH:4][CH:5]=[CH:6][C:7]2=3)[CH2:22]1)([CH3:20])[CH3:19]

Komponenten

6

Edukt 4

HCID 962WaterHCID 10308IminodibenylHCID 24533Sodium amideHCID 128324802-(Chloromethyl)-4-(propan-2-yl)morpholine

Produkt 1

HCID 214427915-(4-isopropyl-2-morpholinylmethyl)-10,11-dihydro-5H-dibenz[b,f]azepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel3×

Versuchsvorschrift

To a suspension of sodium amide (0.5 g) in benzene was added a solution of 10,11-dihydro-5H-dibenz[b,f]azepine (1.0 g) in benzene at room temperature, and the resulting mixture was stirred under reflux for 1 hour. After cooling, a solution of 4-isopropyl-2-chloromethylmorpholine (1.0 g) in benzene was added to the reaction mixture at room temperature, and the resulting mixture was stirred at room temperature for 1 hour and refluxed for 20 hours with stirring. The reaction mixture was cooled and admixed with water. The benzene layer was separated, washed with water, dried over anhydrous magnesium sulfate and evaporated to afford 5-(4-isopropyl-2-morpholinylmethyl)-10,11-dihydro-5H-dibenz[b,f]azepine as an oily substance. M.P. 203.5° -- 204.5° C (oxalate).

Aufarbeitung

  1. temperatureunder reflux for 1 hour
  2. temperatureAfter cooling
  3. stirringthe resulting mixture was stirred at room temperature for 1 hour
  4. temperaturerefluxed for 20 hours
  5. stirringwith stirring
  6. temperatureThe reaction mixture was cooled
  7. customThe benzene layer was separated
  8. washwashed with water
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-8cadcf62a44d4ee4ba6e649edb8b39cf
Quelldatensatz
uspto-grants-1977_04
Patentnummer
US04017621

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