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Acetic Acid → 4-(6-Hexanamido-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl)-3-hydroxybenzoic acid

HRID 1646366
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1646366
C([Li:5])CCC.[CH2:6]([SH:8])[CH3:7].[C:9]([NH:16][C:17]1[CH:18]=[CH:19][C:20]2[O:25][CH2:24][CH2:23][N:22]([CH2:26][C:27]3[CH:36]=[CH:35][C:30]([C:31]([O:33]C)=[O:32])=[CH:29][C:28]=3[O:37]C)[C:21]=2[CH:39]=1)(=[O:15])[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].C(O)(=O)C>CN1C(=O)N(C)CCC1.O>[S-:8][CH2:6][CH3:7].[Li+:5].[C:9]([NH:16][C:17]1[CH:18]=[CH:19][C:20]2[O:25][CH2:24][CH2:23][N:22]([CH2:26][C:27]3[CH:36]=[CH:35][C:30]([C:31]([OH:33])=[O:32])=[CH:29][C:28]=3[OH:37])[C:21]=2[CH:39]=1)(=[O:15])[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]
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Komponenten

8

Edukt 4

HCID 176Acetic AcidHCID 6343EthanethiolHCID 23365905Methyl 4-(6-hexanamido-2,3-dihydrobenz-1,4-oxazin-4ylmethyl)-3-methoxybenzoateHCID 178418339Butyllithium

Produkt 2

HCID 10866251Lithium thioethoxideHCID 23365893
4-(6-Hexanamido-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl)-3-hydroxybenzoic acid
Ausbeute 36 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-Lösungsmittel2×

Versuchsvorschrift

Lithium thioethoxide was prepared by the dropwise addition of n-butyllithium (4 ml. of 1.53 molar solution in hexane) to a stirred solution of ethyl mercaptan (0.5 ml.) in dry N,N'-dimethylpropylene urea (DMPU) (9 ml.), under a nitrogen atmosphere. A solution of methyl 4-(6-hexanamido-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl)-3-methoxybenzoate (prepared as described in Example 26) (0.35 g.) in DMPU (3 ml.) was added, the mixture stirred at ambient temperature for 15 minutes, then heated to, and maintained at, 130° C. for 4 hours. The cooled mixture was diluted with water, acidified with acetic acid, extracted with ethyl acetate, the extracts washed with water, dried (MgSO4) and evaporated. The product was purified by flash chromatography on silica gel, eluting with 80:20:2 v/v/v toluene:ethyl acetate:acetic acid, giving a white solid which was washed with hexane and dried, to give the title compound (0.114 g., 36%) as a white solid, m.p. 183°-184° C.

Aufarbeitung

  1. temperatureheated to, and
  2. temperaturemaintained at, 130° C. for 4 hours
  3. extractionextracted with ethyl acetate
  4. washthe extracts washed with water
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe product was purified by flash chromatography on silica gel
  8. washeluting with 80:20:2 v/v/v toluene
  9. customethyl acetate:acetic acid, giving a white solid which
  10. washwas washed with hexane
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-258c389889d54c909ce2379fa7b49020
Quelldatensatz
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05179112

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