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Methanol → (S)-2-[4-[[3,5-difluoro-4-[(S)-1-methoxycarbonyl-2-[4-[1,3,6-trimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl]phenyl]ethylcarbamoyl]benzylamino]methyl]-2,6-difluorobenzoylamino]-3-[4-[1,3,6-trimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl]phenyl]propionic acid methyl ester

HRID 63753
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 63753
[F:1][C:2]1[CH:3]=[C:4]([CH:41]=[C:42]([F:69])[C:43]=1[C:44](=[O:68])[NH:45][C@H:46]([C:65]([OH:67])=[O:66])[CH2:47][C:48]1[CH:53]=[CH:52][C:51]([C:54]2[C:55](=[O:64])[N:56]([CH3:63])[C:57](=[O:62])[N:58]([CH3:61])[C:59]=2[CH3:60])=[CH:50][CH:49]=1)[CH2:5][NH:6][CH2:7][C:8]1[CH:38]=[C:37]([F:39])[C:11]([C:12]([NH:14][C@@H:15]([CH2:19][C:20]2[CH:25]=[CH:24][C:23]([C:26]3[C:27](=[O:36])[N:28]([CH3:35])[C:29](=[O:34])[N:30]([CH3:33])[C:31]=3[CH3:32])=[CH:22][CH:21]=2)[C:16](O)=[O:17])=[O:13])=[C:10]([F:40])[CH:9]=1.[CH3:70][OH:71].[CH3:72]C(=O)OCC>C(Cl)Cl>[CH3:70][O:71][C:16](=[O:17])[C@@H:15]([NH:14][C:12](=[O:13])[C:11]1[C:37]([F:39])=[CH:38][C:8]([CH2:7][NH:6][CH2:5][C:4]2[CH:3]=[C:2]([F:1])[C:43]([C:44](=[O:68])[NH:45][C@H:46]([C:65]([O:67][CH3:72])=[O:66])[CH2:47][C:48]3[CH:49]=[CH:50][C:51]([C:54]4[C:55](=[O:64])[N:56]([CH3:63])[C:57](=[O:62])[N:58]([CH3:61])[C:59]=4[CH3:60])=[CH:52][CH:53]=3)=[C:42]([F:69])[CH:41]=2)=[CH:9][C:10]=1[F:40])[CH2:19][C:20]1[CH:21]=[CH:22][C:23]([C:26]2[C:27](=[O:36])[N:28]([CH3:35])[C:29](=[O:34])[N:30]([CH3:33])[C:31]=2[CH3:32])=[CH:24][CH:25]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 887MethanolHCID 8857Ethyl AcetateHCID 89720667HCID 89720667, Verbindung

Produkt 1

HCID 89720945(S)-2-[4-[[3,5-difluoro-4-[(S)-1-methoxycarbonyl-2-[4-[1,3,6-trimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl]phenyl]ethylcarbamoyl]benzylamino]methyl]-2,6-difluorobenzoylamino]-3-[4-[1,3,6-trimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl]phenyl]propionic acid methyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a flask containing (S)-2-[4-[[3,5-difluoro-4-[(S)-1-carboxy-2-[4-[1,3,6-trimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl]phenyl]ethylcarbamoyl]benzylamino]methyl]-2,6-difluorobenzoylamino]-3-[4-[1,3,6-trimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl]phenyl]propionic acid (560 mg, 0.59 mmol) was added methanol (50 mL) and TMSCI (398 mg, 460 mL, 3.66 mmol) and the reaction was stirred overnight. Reaction was diluted with EA (10 mL), DCM (140 mL) and was washed with aqueous NaHCO3 solution (water:saturated solution 50 mL:50 mL, 10 mL brine) and brine (100 mL). The organic layer was dried over MgSO4, filtered and concentrated yielding the title compound as a white solid and used directly as is. ES(+)-LRMS m/e calcd. for C50H49F4N7O10 (M+H)+ 984, obsd 984.

Aufarbeitung

  1. customReaction
  2. washwas washed with aqueous NaHCO3 solution (water:saturated solution 50 mL:50 mL, 10 mL brine) and brine (100 mL)
  3. dry with materialThe organic layer was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-480e5d06b1d7486a9f70f80e9cb70cf2
Quelldatensatz
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09447035B2

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