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Triethylamine → methyl 12-[5-amino-3-methyl-2-[3-[5-[N-[(2-methylpropan-2-yl)oxycarbonyl]carbamimidoyl]-2-methylsulfanylthiophen-3-yl]sulfonylphenyl]anilino]-12-oxododecanoate

HRID 2216205
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2216205
C(N(CC)CC)C.[C:8]([O:12][C:13](=[O:44])[NH:14][C:15]([C:17]1[S:18][C:19]([S:42][CH3:43])=[C:20]([S:22]([C:25]2[CH:26]=[C:27]([C:31]3[C:36]([NH2:37])=[CH:35][C:34]([N+:38]([O-])=O)=[CH:33][C:32]=3[CH3:41])[CH:28]=[CH:29][CH:30]=2)(=[O:24])=[O:23])[CH:21]=1)=[NH:16])([CH3:11])([CH3:10])[CH3:9].[CH2:45]([O:47][C:48](=[O:62])[CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][C:59](Cl)=[O:60])C.C([O-])(O)=O.[Na+].[NH4+].[Cl-]>C(Cl)Cl.[Cl-].[Na+].O.CCO.[Fe].CCOC(C)=O>[CH3:45][O:47][C:48](=[O:62])[CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][C:59](=[O:60])[NH:37][C:36]1[CH:35]=[C:34]([NH2:38])[CH:33]=[C:32]([CH3:41])[C:31]=1[C:27]1[CH:28]=[CH:29][CH:30]=[C:25]([S:22]([C:20]2[CH:21]=[C:17]([C:15]([NH:14][C:13]([O:12][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:44])=[NH:16])[S:18][C:19]=2[S:42][CH3:43])(=[O:24])=[O:23])[CH:26]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 5

HCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 516892Sodium BicarbonateHCID 434365111-Ethoxycarbonyldodecanoyl chlorideHCID 145857628tert-butyl N-[4-[3-(2-amino-6-methyl-4-nitrophenyl)phenyl]sulfonyl-5-methylsulfanylthiophene-2-carboximidoyl]carbamate

Produkt 1

HCID 145857669
methyl 12-[5-amino-3-methyl-2-[3-[5-[N-[(2-methylpropan-2-yl)oxycarbonyl]carbamimidoyl]-2-methylsulfanylthiophen-3-yl]sulfonylphenyl]anilino]-12-oxododecanoate
Ausbeute 103,5 %

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 23925IronKatalysatorHCID 702EthanolLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

Triethylamine (139 μL, 1 mmol) was added to a solution of {[4-(6′-amino-2′-methyl-4′-nitro-biphenyl-3-sulfonyl)-5-methylsulfanyl-thiophen-2-yl]-imino-methyl}-carbamic acid tert-butyl ester ((Example 295: step h) 118 mg, 0.21 mmol) in DCM (10 mL). 11-chlorocarbonyl-undecanoic acid ethyl ester (73 mg, 0.26 mmol) was added dropwise over 5 min. After 30 minutes of stirring, the reaction was not complete. Additional portions of acid chloride (3×1 eq) were added in a similar manner, until the reaction was complete. Addition of EtOAc (40 mL) followed by aqueous workup with NaHCO3 (2×20 mL) and brine (30 mL) yielded the crude amide (206 mg) as a glass. The residue was dissolved in EtOH (5 mL) and 4M aq NH4Cl (1 mL) was added. Iron powder (165 mg, 3 mmol) was added and the reaction was heated at 75° C. for 1 h. The cooled mixture was filtered through a 0.22 μm filter and solids washed with 5 mL portions of MeOH and EtOAc. Additional EtOAc (80 mL) was added and the organic solution was washed with citric acid (2×20 mL), NaHCO3 (2×30 mL), water (30 mL), and brine (50 mL). Drying and concentration of the solution yielded the title compound (165 mg) which was used without further purification.

Aufarbeitung

  1. customyielded the crude amide (206 mg) as a glass
  2. filtrationThe cooled mixture was filtered through a 0.22 μm
  3. filtrationfilter
  4. washsolids washed with 5 mL portions of MeOH and EtOAc
  5. additionAdditional EtOAc (80 mL) was added
  6. washthe organic solution was washed with citric acid (2×20 mL), NaHCO3 (2×30 mL), water (30 mL), and brine (50 mL)
  7. customDrying

Quellen und Nachweise

ORD-Eintrag
ord-5e9e5d0f583e44b2a18e2b973965dd9c
Quelldatensatz
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07109354B2

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