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Dimethylformamide dimethyl acetal → tert-Butyl 4-{5-[2-(methylamino)pyrimidin-4-yl]-4-phenyl-1H-imidazol-1-yl}piperidine-1-carboxylate

HRID 1896662
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1896662
[C:1]([C:4]1[N:8]([CH:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)[CH:7]=[N:6][C:5]=1[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)(=O)[CH3:2].C(C1[N:35]([CH:36]2CN(C(OC(C)(C)C)=O)C2)[CH:34]=[N:33][C:32]=1C1C=CC(F)=CC=1)(=O)C.[NH2:54]C1CCN(C(OC(C)(C)C)=O)CC1.[N+](C(C1C=CC=CC=1)S(C1C=CC(C)=CC=1)(=O)=O)#[C-].FC1C=CC(C([N+]#[C-])S(C2C=CC(C)=CC=2)(=O)=O)=CC=1.COC(OC)N(C)C.[Na].Cl.CNC(N)=N.C[O-].[Na+]>O.CO>[CH3:36][NH:35][C:34]1[N:54]=[C:1]([C:4]2[N:8]([CH:9]3[CH2:10][CH2:11][N:12]([C:15]([O:17][C:18]([CH3:19])([CH3:20])[CH3:21])=[O:16])[CH2:13][CH2:14]3)[CH:7]=[N:6][C:5]=2[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:2]=[CH:32][N:33]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

12

Edukt 9

HCID 78373Dimethylformamide dimethyl acetalHCID 12682914-Amino-1-Boc-piperidineHCID 5360545SodiumHCID 10827289a-Tosyl-(4-fluorobenzyl) isocyanideHCID 10942334Sodium MethoxideHCID 10967613a-Tosylbenzyl isocyanide
HCID 57461730
tert-Butyl 3-[5-acetyl-4-(4-fluorophenyl)-1H-imidazol-1-yl]azetidine-1-carboxylate
HCID 58235101tert-butyl 4-(5-acetyl-4-phenyl-1H-imidazol-1-yl)piperidine-1-carboxylate
HCID 178485118HCID 178485118, Verbindung

Produkt 1

HCID 58235109tert-Butyl 4-{5-[2-(methylamino)pyrimidin-4-yl]-4-phenyl-1H-imidazol-1-yl}piperidine-1-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of tert-butyl 4-(5-acetyl-4-phenyl-1H-imidazol-1-yl)piperidine-1-carboxylate [C24, prepared according to the general procedure for the synthesis of tert-butyl 3-[5-acetyl-4-(4-fluorophenyl)-1H-imidazol-1-yl]azetidine-1-carboxylate (C3) in Example 1, except that tert-butyl 4-aminopiperidine-1-carboxylate was used in place of tert-butyl 3-aminoazetidine-1-carboxylate, and 1-{[isocyano(phenyl)methyl]sulfonyl}-4-methylbenzene (C21) was employed rather than 1-fluoro-4-{isocyano[(4-methylphenyl)sulfonyl]methyl}benzene (C2)] (414 mg, 1.12 mmol) and N,N-dimethylformamide dimethyl acetal (4 mL) was heated to 100° C. for 18 hours, then cooled and concentrated in vacuo. The residue was dissolved in anhydrous methanol (2 ml) and added to a solution of N-methylguanidine in methanol [prepared by reacting sodium metal (70 mg, 3 mmol) with anhydrous methanol (2 mL), then adding N-methylguanidine hydrochloride (413 mg, 3.77 mmol) to the resulting sodium methoxide solution]. The reaction mixture was heated at 50° C. for 21 hours, then cooled to room temperature and treated with water (1 mL). The solids were collected by filtration, rinsed with saturated aqueous sodium bicarbonate solution and water and dried to provide the product as a light tan solid. Yield: 230 mg, 0.53 mmol, 47%. APCI m/z 435.0 (M+1). 1H NMR (400 MHz, CDCl3) δ 1.49 (s, 9H), 1.82-1.93 (m, 2H), 2.19 (br d, J=12 Hz, 2H), 2.73-2.82 (m, 2H), 3.06 (d, J=5.1 Hz, 3H), 4.26-4.35 (m, 2H), 4.81-4.90 (m, 1H), 5.16-5.21 (m, 1H), 6.45 (d, J=5.1 Hz, 1H), 7.28-7.34 (m, 3H), 7.48-7.51 (m, 2H), 7.75 (s, 1H), 8.15 (br d, J=4.9 Hz, 1H).

Aufarbeitung

  1. customprepared
  2. temperaturecooled
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in anhydrous methanol (2 ml)
  5. additionadded to a solution of N-methylguanidine in methanol [
  6. customprepared
  7. temperatureThe reaction mixture was heated at 50° C. for 21 hours
  8. temperaturecooled to room temperature
  9. filtrationThe solids were collected by filtration
  10. washrinsed with saturated aqueous sodium bicarbonate solution and water
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d3982063a6af4309867da9f29a576f42
Quelldatensatz
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08518944B2

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