1-Pyrenebutanoic acid → HCID 18459595, 화합물

HRID 2302133

반응식

HRID 2302133 반응식
[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

참가 물질

5

반응물 3

HCID 769771-Pyrenebutanoic acidHCID 80170N-HydroxysuccinimideHCID 22046199HCID 22046199, 화합물

생성물 1

HCID 18459595HCID 18459595, 화합물수율 70%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
0 °C

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-240cf8c13a6e4ae7871d5a2874f03dd3
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06432632B1

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