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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 44242067, Verbindung

HRID 1446055
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1446055
[F:1][C:2]1[CH:3]=[C:4]([N:38]2[CH2:42][C@H:41]([CH2:43][NH:44][C:45](=[O:47])[CH3:46])[O:40][C:39]2=[O:48])[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:37])[CH2:15][O:16][C:17]2[CH:22]=[CH:21][C:20]([CH2:23][O:24][CH:25]3[CH2:30][O:29][C:28]4=[N:31][C:32]([N+:34]([O-:36])=[O:35])=[CH:33][N:27]4[CH2:26]3)=[CH:19][CH:18]=2)[CH2:10][CH2:9]1.C(OC(=O)COC1C=CC(CO[C@@H]2COC3=NC([N+]([O-])=O)=CN3C2)=CC=1)(C)(C)C.FC1C=C(N2CC(CNC(=O)C)OC2=O)C=CC=1N1CCNCC1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.CCN(C(C)C)C(C)C>C(O)(C(F)(F)F)=O.C(Cl)Cl.C(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]([N:38]2[CH2:42][C@H:41]([CH2:43][NH:44][C:45](=[O:47])[CH3:46])[O:40][C:39]2=[O:48])[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:9][CH2:10][N:11]([C:14](=[O:37])[CH2:15][O:16][C:17]2[CH:18]=[CH:19][C:20]([CH2:23][O:24][C@@H:25]3[CH2:30][O:29][C:28]4=[N:31][C:32]([N+:34]([O-:36])=[O:35])=[CH:33][N:27]4[CH2:26]3)=[CH:21][CH:22]=2)[CH2:12][CH2:13]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 18939356N-[[3-(3-Fluoro-4-(piperazin-1-YL)phenyl)-2-oxooxazolidin-5-YL]methyl]acetamideHCID 68545750HCID 68545750, VerbindungHCID 68549864
HCID 68549864, Verbindung

Produkt 1

HCID 44242067HCID 44242067, VerbindungAusbeute 4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 21863450Trifluoroacetic acid methylene chlorideLösungsmittel

Versuchsvorschrift

(S)—N-{3-[3-Fluoro-4-(4-{2-[4-(2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazin-6-yloxymethyl)-phenoxy]-acetyl}-piperazin-1-yl)-phenyl]-2-oxo-oxazolidin-5-ylmethyl}-acetamide. A solution of [4-(2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazin-6(S)-yloxylmethyl)-phenoxy]-acetic acid tert-butyl ester (100 mg, 0.25 mmol) in TFA/CH2Cl2 (2 mL) was stirred at room temperature for 2 h. The resultant mixture was concentrated in vacuo, and diluted with DCM, to the solution was added N-[3-(3-fluoro-4-piperazin-1-yl-phenyl)-2-oxo-oxazolidin-5-ylmethyl]-acetamide (50 mg, 0.15 mmol) (prepared by following the procedure disclosed by U.S. Pat. No. 5,547,950 or Brickner 1996), HOBt (21.6 mg, 0.16 mmol), EDCI (30.7 mg, 0.16 mmol) and DIPEA (0.20 ml). The mixture was stirred at room temperature for 24 hours diluted with DCM, washed with sat. NaHCO3, 1 N HCl and sat. NaHCO3, dried over sodium sulfate, and concentrated in vacuo. The crude product was purified by preparative TLC plates (5% MeOH in dichloromethane) to give the title product as a solid (6.0 mg, 4%). ESI MS m/z 668.4 (M+H+).

Aufarbeitung

  1. concentrationThe resultant mixture was concentrated in vacuo
  2. additiondiluted with DCM, to the solution
  3. customprepared
  4. washwashed with sat. NaHCO3, 1 N HCl and sat. NaHCO3
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe crude product was purified by preparative TLC plates (5% MeOH in dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-ecea4fecde974d2aa381629b03466048
Quelldatensatz
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07666864B2

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