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Phenol → 1-Acetyl-6-bromo-5-[(1,2,3,5,6,8a-hexahydroindolizin-7-yl)methoxy]indoline

HRID 1274236
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1274236
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([OH:14])=[C:10]([Br:13])[CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[CH2:15]1[CH:23]2[N:18]([CH2:19][CH2:20][C:21]([CH2:24]O)=[CH:22]2)[CH2:17][CH2:16]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O.C1(O)C=CC=CC=1>C1COCC1.C(OCC)(=O)C>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([O:14][CH2:24][C:21]3[CH2:20][CH2:19][N:18]4[CH:23]([CH:22]=3)[CH2:15][CH2:16][CH2:17]4)=[C:10]([Br:13])[CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]
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Komponenten

8

Edukt 5

HCID 996PhenolHCID 11776Triphenylphosphine2×HCID 220568ethyl N-ethoxycarbonyliminocarbamate2×HCID 219483801-(6-Bromo-5-hydroxy-2,3-dihydro-1H-indol-1-yl)ethan-1-oneHCID 221209331,2,3,5,6,8a-Hexahydroindolizine-7-methanol

Produkt 1

HCID 22120926
1-Acetyl-6-bromo-5-[(1,2,3,5,6,8a-hexahydroindolizin-7-yl)methoxy]indoline
Ausbeute 13,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

1-Acetyl-6-bromo-5-hydroxyindoline (Tetrahedron, 1973, 29(8), 1115) (1.24 g, 4.8 mmol), 1,2,3,5,6,8a-hexahydroindolizine-7-methanol (D2, 0.74 g, 4.8 mmol) and triphenylphosphine (1.27 g, 4.8 mmol) were stirred under Ar in dry THF (50 ml) as diethyl azodicarboxylate (0.76 ml, 4.8 mmol) was added dropwise. The mixture was stirred for 1 h, diluted with ethyl acetate, and extracted with dil. HCl. The extract was basified with potassium carbonate, and extracted with chloroform. This extract was dried (Na2SO4) and evaporated to give a dark oil. Further treatment of this oil as above with the phenol, triphenylphosphine and diethyl azodicarboxylate caused reaction to proceed further. Chromatography on silica, eluting with 0-20% methanol/dichloromethane, gave the title compound (0.25 g, 13%) as a brown gum.

Aufarbeitung

  1. additionwas added dropwise
  2. extractionextracted with dil. HCl
  3. extractionextracted with chloroform
  4. dry with materialThis extract was dried (Na2SO4)
  5. customevaporated
  6. customto give a dark oil
  7. customreaction
  8. washChromatography on silica, eluting with 0-20% methanol/dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-72d97894ddc44ef3a5690cf2bd344327
Quelldatensatz
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06156783

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