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Acetic Acid → HCID 57971654, Verbindung

HRID 2360670
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2360670
[C:1]([O:5][C:6](=[O:31])[C@@H:7]([NH:14][CH2:15][CH:16]1[CH2:21][CH2:20][CH:19]([CH2:22][NH:23]C(OC(C)(C)C)=O)[CH2:18][CH2:17]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].[CH2:32]([O:36][CH:37]([O:39][NH:40][C:41]([C:43]1[S:47][C:46]2[CH:48]=[C:49]([CH:52]=O)[CH:50]=[CH:51][C:45]=2[CH:44]=1)=[O:42])[CH3:38])[CH:33]([CH3:35])[CH3:34].C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([O-])(O)=O.[Na+]>ClCCCl.C(Cl)Cl>[C:1]([O:5][C:6](=[O:31])[C@@H:7]([NH:14][CH2:15][CH:16]1[CH2:17][CH2:18][CH:19]([CH2:22][NH:23][CH2:52][C:49]2[CH:50]=[CH:51][C:45]3[CH:44]=[C:43]([C:41](=[O:42])[NH:40][O:39][CH:37]([O:36][CH2:32][CH:33]([CH3:34])[CH3:35])[CH3:38])[S:47][C:46]=3[CH:48]=2)[CH2:20][CH2:21]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:4])([CH3:2])[CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 176Acetic AcidHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 57971603HCID 57971603, VerbindungHCID 57971713HCID 57971713, Verbindung

Produkt 1

HCID 57971654HCID 57971654, Verbindung
Ausbeute 34 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 111,2-DichloroethaneLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

(S)-{[4-(tert-Butoxycarbonylamino-methyl)-cyclohexylmethyl]-amino}-phenyl-acetic acid tert-butyl ester (290 mg, 0.9 mmol) and 6-formyl-benzo[b]thiophene-2-carboxylic acid (1-isobutoxy-ethoxy) amide (Scheme 7) (255 mg, 0.8 mmol) were stirred in DCE (8 ml) for 30 min. Acetic acid (4 ul, 0.08 mmol) and sodium triacetoxyborohydride (504 mg, 2.4 mmol) were added and the reaction mixture was stirred at r.t. for 1 h30. DCM (5 ml) and a saturated solution of NaHCO3 (10 ml) were added and phases were separated. The aqueous phase was extracted with EtOAc (15 ml). The organics were dried over magnesium sulfate, filtered and concentrated under vacuum. The crude product (543 mg) was purified on column chromatography (5 to 10% MeOH in DCM) to yield the expected pure product (172 mg, 34% yield). LCMS purity 100%, m/z 638 [M++H]+.

Aufarbeitung

  1. customphases were separated
  2. extractionThe aqueous phase was extracted with EtOAc (15 ml)
  3. dry with materialThe organics were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum
  6. customThe crude product (543 mg) was purified on column chromatography (5 to 10% MeOH in DCM)

Quellen und Nachweise

ORD-Eintrag
ord-00e1105e33d54ca5bfb3d834a1787e06
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08686032B2

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