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Water → methyl 3-(t-butyloxycarbonyl)-1-hydroxymethyl-1,2-dihydro-3H-pyrrolo[3,2-e]indole-7-carboxylate

HRID 366835
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 366835
[C:1]([O:5][C:6]([N:8]1[C:19]2[C:11](=[C:12]3[C:16](=[CH:17][CH:18]=2)[NH:15][C:14]([C:20]([O:22][CH3:23])=[O:21])=[CH:13]3)[CH:10]([CH2:24][O:25]N2C(C)(C)CCCC2(C)C)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].O>C1COCC1.CC(O)=O.[Zn]>[C:1]([O:5][C:6]([N:8]1[C:19]2[C:11](=[C:12]3[C:16](=[CH:17][CH:18]=2)[NH:15][C:14]([C:20]([O:22][CH3:23])=[O:21])=[CH:13]3)[CH:10]([CH2:24][OH:25])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
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Komponenten

6

Edukt 2

HCID 962WaterHCID 10791080methyl 3-(t-butyloxycarbonyl)-1-[(2,2,6,6-tetramethylpiperidino)oxy]methyl-1,2-dihydro-3H-pyrrolo[3,2-e]indole-7-carboxylate

Produkt 1

HCID 10569587methyl 3-(t-butyloxycarbonyl)-1-hydroxymethyl-1,2-dihydro-3H-pyrrolo[3,2-e]indole-7-carboxylateAusbeute 79 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23994ZincKatalysator
HCID 176
Acetic Acid
Lösungsmittel
HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Zinc powder (7.39 g, 113 mmol) was added to a solution of 54 (6.86 g, 14.1 mmol) in THF (150 mL), HOAc (150 mL), and H2O (50 mL). The mixture was stirred at reflux for 40 min, cooled, and filtered through Celite eluting with EtOAc. The filtrate was evaporated and the residue diluted with H2O and extracted with EtOAc (×2). The extracts were washed with H2O, aq NaHCO3, and dried (Na2SO4) and evaporated. Recrystallization from MeOH gave methyl 3-(t-butyloxycarbonyl)-1-hydroxymethyl-1,2-dihydro-3H-pyrrolo[3,2-e]indole-7-carboxylate (55) as a white solid (3.86 g, 79%), mp 189.5-191° C. (dec.). The mother liquor was purified by chromatography (40% EtOAc-petroleum ether) to give more alcohol (0.74 g, 15%). 1H NMR [(CD3)2SO] δ 11.88 (s, 1 H, NH), 7.87 (v br s, 1 H, H-4), 7.29 (d, J=8.9 Hz, 1 H, H-5), 7.11 (d, J=1.4 Hz, 1 H , H-8), 4.95 (t, J=5.2 Hz, 1 H, OH), 4.03 (t, J=10.5 Hz, 1 H), 3.92-3.86 (m, 1 H), 3.87 (s, 3 H, CO2Me), 3.82-3.75 (m, 1 H), 3.67 (br s, 1 H), 3.55-3.48 (m, 1 H), 1.51 (s, 9 H, t-Bu); 13C NMR δ 161.6, 151.8, 136.2, 134.6, 127.8, 123.7, 122.6, 113.3, 113.3, 111.3, 105.5, 79.3, 63.1, 51.7, 51.2, 42.2, 28.1. Anal. Calculated for C18H22N2O5 : C, 62.4; H, 6.4; N, 8.1. Found: C, 62.3; H, 6.6; N, 8.3%.

Aufarbeitung

  1. temperatureat reflux for 40 min
  2. temperaturecooled
  3. filtrationfiltered through Celite
  4. washeluting with EtOAc
  5. customThe filtrate was evaporated
  6. additionthe residue diluted with H2O
  7. extractionextracted with EtOAc (×2)
  8. washThe extracts were washed with H2O, aq NaHCO3
  9. dry with materialdried (Na2SO4)
  10. customevaporated
  11. customRecrystallization from MeOH

Quellen und Nachweise

ORD-Eintrag
ord-8fbdbac26cbb4c9a85248fb78bf634d9
Quelldatensatz
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06130237

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