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Morpholine → [2-(4-Benzyloxy-phenyl)-1-morpholin-4-ylmethyl-ethyl]-carbamic acid tert-butyl ester

HRID 278883
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 278883
[C:1]([O:5][C:6]([NH:8][C@H:9]([CH:25]=O)[CH2:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:13][CH:12]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH:27]1[CH2:32][CH2:31][O:30][CH2:29][CH2:28]1.C([BH3-])#N.[Na+]>CO>[C:1]([O:5][C:6](=[O:7])[NH:8][CH:9]([CH2:25][N:27]1[CH2:32][CH2:31][O:30][CH2:29][CH2:28]1)[CH2:10][C:11]1[CH:12]=[CH:13][C:14]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:15][CH:16]=1)([CH3:4])([CH3:2])[CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8083MorpholineHCID 5003444Sodium cyanoborohydrideHCID 7015729Boc-Tyr(Bzl)-aldehyde

Produkt 1

HCID 18711796[2-(4-Benzyloxy-phenyl)-1-morpholin-4-ylmethyl-ethyl]-carbamic acid tert-butyl esterAusbeute 45 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

A solution consisting of 2.86 g (8 mmol) N-tert-butoxycarbonyl-O-benzyl-L-tyrosinal and 0.701 mL (8 mmol) morpholine (Aldrich, Milwaukee, Wis.) in 36 mL methanol containing 1% acetic acid was stirred at 25° C. for 20 minutes, at which time a solution of 1.06 g (16 mmol) sodium cyanotrihydridoborate (Aldrich, Milwaukee, Wis.) in 12 mL methanol was added and the resulting mixture stirred for 24 hours. The reaction was quenched by the addition of 3 M HCl in 3 mL increments until the vigorous bubbling subsided. The mixture was neutralized with saturated NaHCO3 solution then extracted with three 100 mL portions of ethyl acetate. The combined extracts were washed with 100 mL brine, dried over anhydrous sodium sulphate, and evaporated at reduced pressure to give a clear, colorless oil which was chromatographed on a silica gel column using ethyl acetate:hexane, 1:1 as eluant. The A white, waxy solid was recrystallized from 2,2,4-trimethylpentane to give 1.53 g (45%) of [2-(4-benzyloxy-phenyl)-1-morpholin-4-ylmethyl-ethyl]-carbamic acid tert-butyl ester as soft white crystals; mp 98-99° C.

Aufarbeitung

  1. additionwas added
  2. customThe reaction was quenched by the addition of 3 M HCl in 3 mL increments until the
  3. customvigorous bubbling
  4. extractionthen extracted with three 100 mL portions of ethyl acetate
  5. washThe combined extracts were washed with 100 mL brine
  6. dry with materialdried over anhydrous sodium sulphate
  7. customevaporated at reduced pressure
  8. customto give a clear, colorless oil which
  9. customwas chromatographed on a silica gel column
  10. customThe A white, waxy solid was recrystallized from 2,2,4-trimethylpentane

Quellen und Nachweise

ORD-Eintrag
ord-5d84ba92d5334dda9f10ff83ade2668d
Quelldatensatz
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06362174B1

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