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Monobasic potassium phosphate → (6R,7R)-4-(tert-butoxycarbonyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-6-carboxylic acid

HRID 1022617
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1022617
[Cl:1][C:2]1[CH:3]=[C:4]([C@@H:9]2[O:15][CH2:14][CH2:13][N:12]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:11][C@H:10]2[CH:23]=[O:24])[CH:5]=[CH:6][C:7]=1[Cl:8].Cl([O-])=[O:26].[Na+].P([O-])(O)(O)=O.[K+]>CC(=CC)C.C(O)(C)(C)C.C1COCC1.O.C(OCC)(=O)C>[C:19]([O:18][C:16]([N:12]1[CH2:11][C@@H:10]([C:23]([OH:26])=[O:24])[C@H:9]([C:4]2[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=2)[O:15][CH2:14][CH2:13]1)=[O:17])([CH3:20])([CH3:21])[CH3:22]
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Komponenten

9

Edukt 3

HCID 516951Monobasic potassium phosphateHCID 23668197Sodium ChloriteHCID 86663853tert-butyl (6R,7R)-7-(3,4-dichlorophenyl)-6-formyl-1,4-oxazepane-4-carboxylate

Produkt 1

HCID 66975341(6R,7R)-4-(tert-butoxycarbonyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-6-carboxylic acidAusbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 962
Water
Lösungsmittel
HCID 6386tert-ButanolLösungsmittel
HCID 8028TetrahydrofuranLösungsmittel
HCID 8857Ethyl AcetateLösungsmittel
HCID 105532-Methyl-2-buteneLösungsmittel

Versuchsvorschrift

To a mixed solution of tert-butyl (6R,7R)-7-(3,4-dichlorophenyl)-6-formyl-1,4-oxazepane-4-carboxylate (7.3 g) in 2-methyl-2-butene (45 mL), tert-butanol (100 ml) and THF (100 ml) was added dropwise a solution of sodium chlorite (10.58 g) and potassium dihydrogenphosphate (16.38 g) in water (160 ml) under ice-cooling, and the mixture was stirred under ice-cooling for 2 hr. The reaction mixture was diluted with ethyl acetate. The diluted solution was washed with distilled water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (7.0 g).

Aufarbeitung

  1. temperaturecooling
  2. temperaturecooling for 2 hr
  3. washThe diluted solution was washed with distilled water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by silica gel chromatography (hexane/ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-a2154aebb6c4485a92c9525bcfe0c84d
Quelldatensatz
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08722662B2

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