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Sodium hydride → 4-(4-fluoro-2-methyl-1H-indol-5-yloxy)-5-methyl-6-(3-(methylsulfonyl)propoxy)pyrrolo[2,1-f][1,2,4]triazine

HRID 2111778
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2111778
[CH3:1][S:2]([CH2:5][CH2:6][CH2:7][O:8][C:9]1[C:10]([CH3:19])=[C:11]2[N:16]([CH:17]=1)[N:15]=[CH:14][N:13]=[C:12]2[OH:18])(=[O:4])=[O:3].O=P(Cl)(Cl)Cl.[F:25][C:26]1[C:34](O)=[CH:33][CH:32]=[C:31]2[C:27]=1[CH:28]=[C:29]([CH3:36])[NH:30]2.[H-].[Na+]>ClCCl.CN(C=O)C>[F:25][C:26]1[C:34]([O:18][C:12]2[C:11]3=[C:10]([CH3:19])[C:9]([O:8][CH2:7][CH2:6][CH2:5][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:17][N:16]3[N:15]=[CH:14][N:13]=2)=[CH:33][CH:32]=[C:31]2[C:27]=1[CH:28]=[C:29]([CH3:36])[NH:30]2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 24758Sodium hydrideHCID 24813Phosphorus oxychlorideHCID 103520364-fluoro-2-methyl-1H-indol-5-olHCID 178431468HCID 178431468, Verbindung

Produkt 1

HCID 115029124-(4-fluoro-2-methyl-1H-indol-5-yloxy)-5-methyl-6-(3-(methylsulfonyl)propoxy)pyrrolo[2,1-f][1,2,4]triazineAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel

2
HCID 6228DimethylformamideLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

A mixture of 6-(3-methanesulfonyl-propoxy)-5-methylpyrrolo[2,1-f][1,2,4]triazin-4-ol (620 mg, 2.17 mmol) and POCl3 (10 mL) was heated at 85° C. for 3 h. POCl3 was removed in vacuo to give a yellow solid, which was dissolved in dichloromethane, and washed successively with cold NaHCO3 solution and brine. The organics were dried, filtered and concentrated to afford the crude chloroimidate intermediate (610 mg), which was added to a pre-mixed solution of 4-fluoro-2-methyl-1H-indol-5-ol (664 mg, 4.02 mmol) and NaH (60% in mineral oil, 160 mg, 4.02 mmol) in DMF at 0° C. The resulting mixture was stirred at RT for 30 min, and diluted with dichloromethane, washed with 10% LiCl aqueous solution, dried concentrated. The residue was purified by flash column chromatography (silica gel, eluting from 10% ethyl acetate/dichloromethane to 30% ethyl acetate/dichloromethane). The desired fractions were combined and concentrated in vacuo to give a solid, which was washed with MeOH to afford the title compound as a white solid (610 mg, 65% yield). HRMS (M+H)+ Calcd. For C20H21FN4O4S: 432.12675. Found: 433.1329. 1H NMR (d-DMSO)δ 11.36 (br, 1H), 7.94 (s, 1H), 7.93 (s, 1H), 7.15 (d, 1H, J=8.4 Hz), 6.99 (m, 1H), 6.24 (s, 1H), 4.16 (t, 2H, J=6.16 Hz), 3.31 (t, 2H, J=5.7 Hz), 3.05 (s, 3H), 2.42 (s, 3H), 2.41 (s, 3H), 2.50 (m, 2H). Anal. Calcd. For C20H21FN4O4S: 0.4 H2O: C 54.58; H 4.84; N 12.56; S 7.29. Found: C 54.61; H 4.92; N 12.65; S 7.33.

Aufarbeitung

  1. customPOCl3 was removed in vacuo
  2. customto give a yellow solid, which
  3. washwashed successively with cold NaHCO3 solution and brine
  4. customThe organics were dried
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto afford the crude chloroimidate intermediate (610 mg), which
  8. washwashed with 10% LiCl aqueous solution
  9. customdried
  10. concentrationconcentrated
  11. customThe residue was purified by flash column chromatography (silica gel, eluting from 10% ethyl acetate/dichloromethane to 30% ethyl acetate/dichloromethane)
  12. concentrationconcentrated in vacuo
  13. customto give a solid, which
  14. washwas washed with MeOH

Quellen und Nachweise

ORD-Eintrag
ord-16a09e81876c4849b4f121d18d58d95f
Quelldatensatz
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07521450B2

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