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4-Pentylaniline → HCID 67396887, Verbindung

HRID 914514
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 914514
[C:1]([CH2:4][C:5]1[N:6]=[C:7]([S:10][C:11]([CH3:16])([CH3:15])[C:12]([OH:14])=[O:13])[S:8][CH:9]=1)(O)=O.[CH2:17]([C:22]1[CH:28]=[CH:27][C:25]([NH2:26])=[CH:24][CH:23]=1)[CH2:18][CH2:19][CH2:20][CH3:21]>O1CCCC1>[CH3:15][C:11]([S:10][C:7]1[S:8][CH:9]=[C:5]([CH2:4][CH2:1][NH:26][C:25]2[CH:27]=[CH:28][C:22]([CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[CH:23][CH:24]=2)[N:6]=1)([CH3:16])[C:12]([OH:14])=[O:13]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 931624-PentylanilineHCID 67399201HCID 67399201, Verbindung

Produkt 1

HCID 67396887HCID 67396887, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

An operation similar to that of Example 520-1 was performed using 2-{[4-(carboxymethyl)-1,3-thiazol-2-yl]thio}-2-methylpropionic acid resin synthesized in Example 461-4 and 4-amylaniline (0.098 g) as starting materials. To the obtained resin were added tetrahydrofuran (2.0 mL) and 1 mol/L borane-tetrahydrofuran complex (2.0 mL), and the mixture was stirred at room temperature overnight. The resin was collected by filtration from the reaction mixture, washed once with tetrahydrofuran, twice with tetrahydrofuran/methanol=1:1 solution, and twice with methanol. Then, a solution (4.0 mL) of tetrahydrofuran-methanol-piperidine (1:1:2) was added to the resin, and the mixture was stirred at room temperature overnight. After completion of the reaction, the resin was collected by filtration, washed four times with tetrahydrofuran and twice with methanol, and vacuum dried to give the title pale-yellow resin (0.30 g).

Aufarbeitung

  1. filtrationThe resin was collected by filtration from the reaction mixture
  2. washwashed once with tetrahydrofuran, twice with tetrahydrofuran/methanol=1:1 solution
  3. additionThen, a solution (4.0 mL) of tetrahydrofuran-methanol-piperidine (1:1:2) was added to the resin
  4. stirringthe mixture was stirred at room temperature overnight
  5. customAfter completion of the reaction
  6. filtrationthe resin was collected by filtration
  7. washwashed four times with tetrahydrofuran
  8. dry with materialtwice with methanol, and vacuum dried

Quellen und Nachweise

ORD-Eintrag
ord-0d9b47ecf33d4e9a96e7fafa3c408767
Quelldatensatz
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08026370B2

Notizen zur Reaktion

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