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Sodium borohydride → (3-(3,4-Dimethoxyphenyl)-5-oxopyrrolidin-3-yl)acetic acid ethyl ester

HRID 343491
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 343491
[CH2:1]([O:3][C:4](=[O:25])[CH2:5][C:6]([C:23]#[N:24])([C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([O:21][CH3:22])[CH:14]=1)[CH2:7][C:8](OCC)=[O:9])[CH3:2].[BH4-].[Na+].C(OCC)(=O)C.CO>CO.O.O.O.O.O.O.[Co](Cl)Cl>[CH2:1]([O:3][C:4](=[O:25])[CH2:5][C:6]1([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([O:21][CH3:22])[CH:14]=2)[CH2:7][C:8](=[O:9])[NH:24][CH2:23]1)[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 4311764Sodium borohydrideHCID 153920193-Cyano-3-(3,4-dimethoxyphenyl)pentanedioic diethyl esterHCID 21584119Ethylacetate methanol

Produkt 1

HCID 15392020(3-(3,4-Dimethoxyphenyl)-5-oxopyrrolidin-3-yl)acetic acid ethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 517166Dichlorocobalt hexahydrateKatalysator
HCID 887MethanolLösungsmittel

Versuchsvorschrift

Combine 3-cyano-3-(3,4-dimethoxyphenyl)pentanedioic diethyl ester (1.3 g, 3.24 mmol) and cobalt(II)chloride hexahydrate (1.54 g, 6.48 mmol) in methanol (50 mL). While maintaining the temperature at or below 20° C. with an ice-bath, add portionwise sodium borohydride (2.17 g, 57 mmol). After the addition is complete, allow the reaction mixture to stand at ambient temperature for 18 hours. Evaporate the reaction mixture invacuo to obtain a residue. Partition the residue between dichloromethane and 1M hydrochloric acid solution. Extract the aqueous layer several times with dichloromethane, combine the organic layers, dry over Na2SO4, filter, and concentrate invacuo to obtain a residue. Chromatograph the residue on silica gel eluting with 20/1 ethyl acetate/methanol. Remove residual solvent inuacuo at 82° C. to give the title compound: Rf= 0.74 (silica gel, 5/1 ethyl acetate/methanol); mp; 116°-118° C. Elemental Analysis calculated for C16H21NO5 : C 62.53; H 6.89; N 4.56; Found: C 62.52; H 6.85; N 4.50.

Aufarbeitung

  1. temperatureWhile maintaining the temperature at or below 20° C. with an ice-bath
  2. additionAfter the addition
  3. customEvaporate the reaction mixture invacuo
  4. customto obtain a residue
  5. customPartition the residue between dichloromethane and 1M hydrochloric acid solution
  6. extractionExtract the aqueous layer several times with dichloromethane
  7. dry with materialdry over Na2SO4
  8. filtrationfilter
  9. concentrationconcentrate invacuo
  10. customto obtain a residue
  11. customRemove residual solvent inuacuo at 82° C.

Quellen und Nachweise

ORD-Eintrag
ord-0f26e558cca24a468db03bd81fe9ce8e
Quelldatensatz
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05861417

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