Pyrenebutyrylhydrazine → Pyrene

HRID 895778

반응식

HRID 895778 반응식
[C:1]1(CCCC(NN)=O)[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.OC1O[C@H](CO)[C@@H](O[C@@H]2O[C@H](CO)[C@H](O)[C@H](O)[C@H]2O)[C@H](O)[C@H]1O>CS(C)=O>[CH:8]1[C:7]2[C:16]3=[C:15]4[C:4](=[CH:5][CH:6]=2)[CH:3]=[CH:2][CH:1]=[C:14]4[CH:13]=[CH:12][C:11]3=[CH:10][CH:9]=1

참가 물질

4

반응물 2

HCID 124220PyrenebutyrylhydrazineHCID 440995(+)-Lactose

생성물 1

HCID 31423Pyrene

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
90 °C

실험 절차

10 μl of a solution containing 400 nmol of 1-pyrenebutanoic acid, hydrazide (Molecular Probes) in DMSO was added to 50 nmol of lactose which had been dried adequately, and lactose was fully dissolved by sonication. 1 μl of acetic acid was added thereto and the mixture was stirred adequately. The reaction mixture was then heated at 90° C. for 1 hour. After the reaction mixture was dried using a centrifugation concentrator, 10 μl of a solution containing 2.5 M borane-dimethylamine complex and 30% acetic acid in DMSO was added to the residue, and the residue was fully dissolved by sonication. The mixture was then heated at 80° C. for 1 hour. The reaction mixture was dried using a centrifugation concentrator. The residue was re-dissolved in 50% acetonitrile and purified using normal phase high performance liquid chromatography. The molecular weight of the purified pyrene-labeled lactose was determined using a triple-quadrupole ion-spray mass-spectrometer API-300. As a result, a positive molecular ion (629.3) was observed.

후처리

  1. customhad been dried adequately
  2. dissolutionlactose was fully dissolved by sonication
  3. addition1 μl of acetic acid was added
  4. customAfter the reaction mixture was dried
  5. additioncontaining 2.5 M borane-dimethylamine complex and 30% acetic acid in DMSO
  6. additionwas added to the residue
  7. dissolutionthe residue was fully dissolved by sonication
  8. temperatureThe mixture was then heated at 80° C. for 1 hour
  9. customThe reaction mixture was dried
  10. dissolutionThe residue was re-dissolved in 50% acetonitrile
  11. custompurified

출처 및 근거

ORD 기록
ord-826ed366131548acb6b3e46ab7bfbc01
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06916920B2

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