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Trimethyl borate → HCID 59713649, Verbindung

HRID 2223092
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2223092
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([O:8][CH3:9])[N:3]=1.[Li]CCCC.B(OC)(OC)OC.Cl[C:23]1[C:29]2[CH:30]=[C:31]([Cl:34])[CH:32]=[CH:33][C:28]=2[N:27]([CH3:35])[C:26](=[O:36])[CH2:25][N:24]=1.[F-].[Cs+]>CCOCC.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C(Cl)Cl.O.COCCOC>[Cl:34][C:31]1[CH:32]=[CH:33][C:28]2[N:27]([CH3:35])[C:26](=[O:36])[CH2:25][N:24]=[C:23]([C:2]3[CH:7]=[CH:6][CH:5]=[C:4]([O:8][CH3:9])[N:3]=3)[C:29]=2[CH:30]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 5

HCID 8470Trimethyl borateHCID 25953Cesium fluorideHCID 2568102-Bromo-6-methoxypyridineHCID 123385855,7-Dichloro-1-methyl-1,3-dihydro-2H-1,4-benzodiazepin-2-oneHCID 178418339Butyllithium

Produkt 1

HCID 59713649HCID 59713649, VerbindungAusbeute 57 %

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 178418397HCID 178418397, VerbindungKatalysatorHCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 80711,2-DimethoxyethaneLösungsmittel

Reaktionsbedingungen

Temperatur
-40 °C

Versuchsvorschrift

As illustrated in the scheme above, absolution of 2-bromo-6-methoxypyridine (0.022 mL, 0.18 mmol) in dry Et2O (0.3 mL) was added to a solution of n-BuLi (0.12 mL of 1.6 M in hexanes, 0.19 mmol) maintained at −40° C. The reaction was stirred at −40° C. for 20 min., and then B(OMe)3 (0.022 mL, 0.19 mmol) was added dropwise. The reaction was stirred at −40° C. for 30 min., and then at room temperature for 3.5 h. The reaction was concentrated in vacuo, anhydrous MeOH was added to the residue, and the reaction was concentrated in vacuo once again. Dry DME (0.8 mL), 5,7-dichloro-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one (0.0392 g, 0.161 mmol), Pd(PPh3)4 (0.0093 g, 0.0080 mmol) and CsF (0.0612 g, 0.403 mmol) were added to the residue, and the mixture was heated to reflux for 15 h. Water (5 mL) and CH2Cl2 (5 mL) were added to the reaction mixture, and the layers were separated. The aqueous phase was extracted with additional CH2Cl2 (3×), and the combined organic phases were dried over Na2SO4, filtered, and concentrated in vacuo. Purification of the crude product by silica gel column chromatography (2:1 CH2Cl2:EtOAc) provided the title compound (0.029 g, 57%). 1H-NMR (CDCl3): δ 7.77 (d, J=7.6 Hz, 1H), 7.71-7.64 (m, 2H), 7.49 (dd, J=2.4 Hz, J=8.8 Hz, 1H), 7.27 (d, J=8.8 Hz, 1H), 6.83 (d, J=8.0 Hz, 1H), 4.85 (d, J=10.8 Hz, 1H), 3.86 (d, J=10.4 Hz, 1H), 3.81 (s, 3H), 3.39 (s, 3H). MS (ESI) (M+H)+=316.

Aufarbeitung

  1. stirringThe reaction was stirred at −40° C. for 30 min.
  2. waitat room temperature for 3.5 h
  3. concentrationThe reaction was concentrated in vacuo, anhydrous MeOH
  4. additionwas added to the residue
  5. concentrationthe reaction was concentrated in vacuo once again
  6. temperaturethe mixture was heated
  7. temperatureto reflux for 15 h
  8. customthe layers were separated
  9. extractionThe aqueous phase was extracted with additional CH2Cl2 (3×)
  10. dry with materialthe combined organic phases were dried over Na2SO4
  11. filtrationfiltered
  12. concentrationconcentrated in vacuo
  13. customPurification of the crude product by silica gel column chromatography (2:1 CH2Cl2:EtOAc)

Quellen und Nachweise

ORD-Eintrag
ord-cc77d8070aac449f9b88e202867e4937
Quelldatensatz
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07375101B2

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