Water → HCID 46830651, Verbindung

HRID 1925186Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1925186
[CH3:1][C:2]1([C:8]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[CH:14]=[CH:13][C:12]=2[S:21]C(C2(C)CCCCC2)=O)=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[OH-].[K+].O>CO.O1CCCC1>[SH:21][C:12]1[CH:13]=[CH:14][C:15]2[C:20](=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:11]=1[NH:10][C:8]([C:2]1([CH3:1])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]1)=[O:9]

Komponenten

6

Edukt 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 866429901-methyl-cyclohexanecarbothioic acid S-{1-[(1-methyl-cyclohexanecarbonyl)-amino]-naphthalen-2-yl}ester

Produkt 1

HCID 46830651HCID 46830651, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

The crude product obtained in step A) is dissolved in a mixture of methanol and tetra-hydrofuran (1:1). Then 3.5 mol equivalents of potassium hydroxide are added at room temperature and the mixture is stirred for 1 hour. Then water is added and the mixture is washed with n-hexane. The aqueous layer is then acidified by addition of KHSO4 and extracted with chloroform. The combined extracts are washed with water and brine, dried (Na2SO4) and concentrated to obtain the desired title compound.

Aufarbeitung

  1. washthe mixture is washed with n-hexane
  2. additionThe aqueous layer is then acidified by addition of KHSO4
  3. extractionextracted with chloroform
  4. washThe combined extracts are washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-3b51cccafaf64a3e866cbebfdb909f88
Quelldatensatz
uspto-grants-2012_05
Patentnummer
US08178583B2

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