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Ethanol → (R)-3-[N-(5'-Chloro-2'-fluorobiphenyl-4-ylmethyl)-N'-(2-hydroxythiazole-5-carbonyl)hydrazino]-2-hydroxypropionic Acid

HRID 541505
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 541505
[OH:1][C:2]1[S:3][C:4]([C:7]([OH:9])=O)=[CH:5][N:6]=1.CN(C(ON1N=NC2C=CC(=CC1=2)Cl)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CN(C=O)C.C([O:42][C:43](=[O:64])[C@H:44]([OH:63])[CH2:45][N:46]([CH2:48][C:49]1[CH:54]=[CH:53][C:52]([C:55]2[CH:60]=[C:59]([Cl:61])[CH:58]=[CH:57][C:56]=2[F:62])=[CH:51][CH:50]=1)[NH2:47])C.CCN(C(C)C)C(C)C.CCO.[Li+].[OH-].O>>[Cl:61][C:59]1[CH:58]=[CH:57][C:56]([F:62])=[C:55]([C:52]2[CH:53]=[CH:54][C:49]([CH2:48][N:46]([CH2:45][C@@H:44]([OH:63])[C:43]([OH:64])=[O:42])[NH:47][C:7]([C:4]3[S:3][C:2]([OH:1])=[N:6][CH:5]=3)=[O:9])=[CH:50][CH:51]=2)[CH:60]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 8

HCID 702EthanolHCID 962WaterHCID 3939Lithium HydroxideHCID 6228DimethylformamideHCID 81531DiisopropylethylamineHCID 200616172-Oxo-2,3-dihydro-1,3-thiazole-5-carboxylic acidHCID 42624899
O-(6-Chlorobenzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate
HCID 67972425(R)-3-[N-(5'-Chloro-2'-fluorobiphenyl-4-ylmethyl)hydrazino]-2-hydroxypropionic Acid Ethyl Ester

Produkt 1

HCID 178523955(R)-3-[N-(5'-Chloro-2'-fluorobiphenyl-4-ylmethyl)-N'-(2-hydroxythiazole-5-carbonyl)hydrazino]-2-hydroxypropionic AcidAusbeute 15,7 %

Versuchsvorschrift

2-Hydroxy-5-thiazolecarboxylic acid (43.5 mg, 0.3 mmol) and HCTU (124 mg, 0.3 mmol) were stirred in DMF (1.3 mL, 16.4 mmol) for 15 minutes at room temperature. (R)-3-[N-(5′-Chloro-2′-fluorobiphenyl-4-ylmethyl)hydrazino]-2-hydroxypropionic acid ethyl ester (100 mg, 0.3 mmol) and DIPEA (142 μL, 818 μmol) were added, and resulting mixture was stirred at room temperature for 30 minutes. The mixture was then evaporated under reduced pressure. The residue was dissolved in EtOH (955 μL, 16.4 mmol). A solution of 1.0 M LiOH in water (1.4 mL, 1.4 mmol) was added and the resulting mixture was stirred at 40° C. for 3 hours. LC/MS showed completion. The solvent was removed in vacuo and the residue was purified by preparative HPLC to yield the title compound (22 mg) as a TFA salt. MS m/z [M+H]+ calc'd for C20H17ClFN3O5S, 466.06. found 466.0.

Aufarbeitung

  1. customresulting mixture
  2. customThe mixture was then evaporated under reduced pressure
  3. stirringthe resulting mixture was stirred at 40° C. for 3 hours
  4. customThe solvent was removed in vacuo
  5. customthe residue was purified by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-a2967c70a53744ca81c666d98f23919b
Quelldatensatz
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08871792B2

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