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Triethylamine → 1-(3,3-Dimethyl-butyl)-piperidine-4-carboxylic Acid 2-methyl-4-(2-methyl-4,5-dihydro-1-oxa-3,6-diaza-benzo[e]azulene-6-carbonyl)-benzylamide

HRID 220985
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 220985
Cl.[NH2:2][CH2:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([N:12]2[CH2:21][CH2:20][C:19]3[N:18]=[C:17]([CH3:22])[O:16][C:15]=3[C:14]3[CH:23]=[CH:24][CH:25]=[CH:26][C:13]2=3)=[O:11])=[CH:6][C:5]=1[CH3:27].C(N(CC)CC)C.[CH3:35][C:36]([CH3:49])([CH3:48])[CH2:37][CH2:38][N:39]1[CH2:44][CH2:43][CH:42]([C:45](O)=[O:46])[CH2:41][CH2:40]1.C1CN([P+](Br)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F>ClCCl.CN(C1C=CN=CC=1)C.CCOC(C)=O>[CH3:27][C:5]1[CH:6]=[C:7]([C:10]([N:12]2[CH2:21][CH2:20][C:19]3[N:18]=[C:17]([CH3:22])[O:16][C:15]=3[C:14]3[CH:23]=[CH:24][CH:25]=[CH:26][C:13]2=3)=[O:11])[CH:8]=[CH:9][C:4]=1[CH2:3][NH:2][C:45]([CH:42]1[CH2:43][CH2:44][N:39]([CH2:38][CH2:37][C:36]([CH3:49])([CH3:48])[CH3:35])[CH2:40][CH2:41]1)=[O:46]
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Komponenten

8

Edukt 4

HCID 8471TriethylamineHCID 2733179PyBroPHCID 231123781-(3,3-Dimethylbutyl)piperidine-4-carboxylic acidHCID 67287214(4-Aminomethyl-3-methyl-phenyl)-(2-methyl-4,5-dihydro-1-oxa-3,6-diaza-benzo[e]azulen-6-yl)-methanone Hydrochloride

Produkt 1

HCID 11642392
1-(3,3-Dimethyl-butyl)-piperidine-4-carboxylic Acid 2-methyl-4-(2-methyl-4,5-dihydro-1-oxa-3,6-diaza-benzo[e]azulene-6-carbonyl)-benzylamide
Ausbeute 69 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 6344DichloromethaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

(4-Aminomethyl-3-methyl-phenyl)-(2-methyl-4,5-dihydro-1-oxa-3,6-diaza-benzo[e]azulen-6-yl)-methanone hydrochloride from Example E119.2 (89 mg, 0.225 mmol) was dissolved in dichloromethane (10 ml) and triethylamine (to pH9) at room temperature. 1-(3,3-Dimethyl-butyl)-piperidine-4-carboxylic acid (53 mg, 0.25 mmol), DMAP (27 mg, 0.225 mmol) and PyBroP (165 mg, 0.36 mmol) were added and the mixture was heated at reflux for 18 h. The solution was diluted with EtOAc, washed with saturated NaHCO3 then brine, dried and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (eluant; 1% 35% ammonia:9% methanol:90% dichloro-methane) to give a white solid identified as the title compound (84 mg, 69%).

Aufarbeitung

  1. customat room temperature
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 18 h
  4. washwashed with saturated NaHCO3
  5. dry with materialbrine, dried
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash chromatography on silica gel (eluant; 1% 35% ammonia:9% methanol:90% dichloro-methane)
  8. customto give a white solid

Quellen und Nachweise

ORD-Eintrag
ord-821226f5468f4ed8b752227fa022459e
Quelldatensatz
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08202858B2

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