1-Pyrenebutanoic acid → HCID 18459595, Verbindung

HRID 2302133

Reaktionsgleichung

[C:1]1([CH2:17][CH2:18][CH2:19][C:20]([OH:22])=[O:21])[C:14]2[C:15]3=[C:16]4[C:11](=[CH:12][CH:13]=2)[CH:10]=[CH:9][CH:8]=[C:7]4[CH:6]=[CH:5][C:4]3=[CH:3][CH:2]=1.O[N:24]1[C:28](=[O:29])[CH2:27][CH2:26][C:25]1=[O:30].ClC(N=C=N)CC(Cl)CCC>CS(C)=O>[C:25]1(=[O:30])[N:24]([C:2]2[CH:3]=[C:4]3[C:15]4=[C:16]5[C:11]([CH:10]=[CH:9][CH:8]=[C:7]5[CH:6]=[CH:5]3)=[CH:12][CH:13]=[C:14]4[C:1]=2[CH2:17][CH2:18][CH2:19][C:20]([OH:22])=[O:21])[C:28](=[O:29])[CH2:27][CH2:26]1

Komponenten

Reaktionsbedingungen

Temperatur: 0 °C

Versuchsvorschrift

SPB was prepared according to the synthesis scheme shown in FIG. 2. In 20 ml of dimethylsulfoxide (DMF), 2.25 g of 1-pyrenebutanoic acid (7.8 mmol: obtained from Molecular Probes, Inc.) and 1.2 g of N-hydroxy succinimide (10.4 mmol: obtained from Wako Pure Chemical Industries, Ltd.) were dissolved. After the mixed solution was cooled to 0° C., 2.69 g of 1,3-dichlorohexylcarbodiimide (13.1 mmol: DCC) was added thereto. Then, the mixture was reacted at 0° C. for 24 hours while stirring. After the reacted solution was filtered with a 0.45 μm filter, the filtrate was collected and dried using an evaporator. Then, the filtrate was recrystallized from 95% ethanol, thereby obtaining 1.88 g of succinimidyl-1-pyrenebutanoic acid (yield: 70%).

Aufarbeitung

customSPB was prepared
customaccording to the synthesis scheme
customThen, the mixture was reacted at 0° C. for 24 hours
filtrationAfter the reacted solution was filtered with a 0.45 μm
filtrationfilter
customthe filtrate was collected
customdried
customan evaporator
customThen, the filtrate was recrystallized from 95% ethanol

Quellen und Nachweise

ORD-Eintrag: ord-240cf8c13a6e4ae7871d5a2874f03dd3
Quelldatensatz: uspto-grants-2002_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06432632B1

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