Methyl iodide → HCID 68651293, Verbindung

HRID 1949091Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1949091
[F:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10]1[C:9]([O:15][CH2:16][CH2:17][N:18]([CH3:20])[CH3:19])=[C:8]3[NH:21][C:22]4[CH:23]=[CH:24][C:25]([F:28])=[CH:26][C:27]=4[C:7]3=[CH:6][C:5]2=1.[CH3:29][I:30]>ClCCl>[I-:30].[F:28][C:25]1[CH:26]=[C:27]2[C:22](=[CH:23][CH:24]=1)[NH:21][C:8]1[C:9]([O:15][CH2:16][CH2:17][N+:18]([CH3:29])([CH3:19])[CH3:20])=[C:10]3[NH:11][C:12]4[CH:13]=[CH:14][C:2]([F:1])=[CH:3][C:4]=4[C:5]3=[CH:6][C:7]2=1

Komponenten

4

Edukt 2

HCID 6328Methyl iodideHCID 45138929HCID 45138929, Verbindung

Produkt 1

HCID 68651293HCID 68651293, VerbindungAusbeute 62 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 2-(2,10-difluoro-5,7-dihydroindolo[2,3-b]carbazol-6-yloxy)-N,N-dimethylethanamine (14 mg) in dichloromethane (8 mL) was added MeI (1.0 mL) at RT under Ar. The resultant solution was stirred overnight and the solid formed. The solid was collected by filtration and washed once with dichloromethane and dried under vacuum to give the title compound (12 mg, 62%). 1H NMR (400 MHz, CD3OD) δ ppm 8.51 (s, 1H), 7.84 (dd, T=9.2, 2.8 Hz, 2H), 7.44 (dd, T=8.8, 4.0 Hz, 2H), 7.12 (ddd, J=9.2, 9.6, 2.4 Hz, 2H), 4.75-4.68 (m, 2H), 4.12-4.07 (m, 2H), 3.46 (s, 9H); MS (ESI) e/z 394 (M-I)+.

Aufarbeitung

  1. customthe solid formed
  2. filtrationThe solid was collected by filtration
  3. washwashed once with dichloromethane
  4. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-e4aa9d198dc646e89c5706e8239490ff
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08399502B2

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