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Ethyl 2-(diphenylmethyleneamino)acetate → HCID 23497591, Verbindung

HRID 841048
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 841048
[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[N:8][CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Li+].CC([N-]C(C)C)C.[C:29]1([S:35]([O:38][C:39]2[CH:40]=[CH:41][C:42]([CH2:45]Br)=[N:43][CH:44]=2)(=[O:37])=[O:36])[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>C1COCC1>[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[N:8][CH:9]([CH2:45][C:42]2[CH:41]=[CH:40][C:39]([O:38][S:35]([C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=3)(=[O:37])=[O:36])=[CH:44][N:43]=2)[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 319508Ethyl 2-(diphenylmethyleneamino)acetateHCID 2724682Lithium diisopropylamideHCID 10639974HCID 10639974, Verbindung

Produkt 1

HCID 23497591HCID 23497591, VerbindungAusbeute 72,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

A solution of ethyl N-(diphenylmethylene)glycinate (1.71 g, 6.40 mmol) in dry THF (10 ml) was added to a stirred solution of LDA (2M in heptane/THF/ethylbenzene, 3.20 ml, 6.40 mmol) in dry THF (10 ml) at −70° under nitrogen. After stirring at this temperature for 0.75 h, a solution of 5-benzenesulphonyloxy-2-bromomethyl-pyridine [2.00 g, 6.01 mmol; prepared as described by Myers et al, J.Org.Chem. (1996), 61, 813] in dry THF (10 ml) was added. The reaction mixture was stirred at −70° for 1 h then at room temperature for 18 h. The reaction was quenched with water (10 ml) then partitioned between EtOAc (70 ml) and brine (30 ml). The phases were separated and the aqueous phase re-extracted with EtOAc (2×40 ml). The combined organic extracts were washed with brine (10 ml), dried (Na2SO4) and evaporated in vacuo to afford the crude product as a dark oil. Purification by flash chromatography (silica, 60% to 75% Et2O/hexane; applied as DCM solution) afforded the title compound as a tan-coloured solid (2.25 g, 72%). δH (CDCl3) 8.02 (1H, d, J 2.8 Hz, pyr-H(6), 7.72 (2H, d, J˜8 Hz, ortho-Ar—H), 7.59 (1H, t, J˜8 Hz, para-Ar—H), 7.50 (2H, dd, J 8.4, 1.4 Hz, phenyl-H), 7.40-7.27 (8H, ms, Ar and phenyl-H), 7.19 (1H, dd, J 8.5, 2.8 Hz, pyr-H(4), 7.11 (1H, d, J 8.5 Hz, pyr-H(3), 6.67 (2H, br d, J˜8 Hz, phenyl-H), 4.50 (1H, dd, J 9, 4.6 Hz, CH-α), 4.24-4.10 (2H, sym.m. CH2CH3), 3.50-3.33 (2H, m, pyr-CH2), 1.24 (3H, t, J 7.2 Hz, CH2CH3); m/z (ESI) 515 (MH+).

Aufarbeitung

  1. stirringThe reaction mixture was stirred at −70° for 1 h
  2. waitat room temperature for 18 h
  3. customThe reaction was quenched with water (10 ml)
  4. customthen partitioned between EtOAc (70 ml) and brine (30 ml)
  5. customThe phases were separated
  6. extractionthe aqueous phase re-extracted with EtOAc (2×40 ml)
  7. washThe combined organic extracts were washed with brine (10 ml)
  8. dry with materialdried (Na2SO4)
  9. customevaporated in vacuo
  10. customto afford the crude product as a dark oil
  11. customPurification by flash chromatography (silica, 60% to 75% Et2O/hexane; applied as DCM solution)

Quellen und Nachweise

ORD-Eintrag
ord-d7b4cc7fafce451a9463486c8a628a74
Quelldatensatz
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06369229B1

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