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Methanesulfonic Acid → HCID 66835135, 화합물

HRID 2275286
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HRID 2275286 반응식
O[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]1[CH2:17][C:16]2[C:11](=[CH:12][C:13]([O:18][CH3:19])=[CH:14][CH:15]=2)[C:10]([CH3:21])([CH3:20])[C:9]1=[O:22].CS(O)(=O)=O.[OH-].[Na+]>>[CH3:19][O:18][C:13]1[CH:14]=[CH:15][C:16]2[CH2:17][C:8]3[C:7]4[CH:2]=[CH:3][N:4]=[CH:5][C:6]=4[O:22][C:9]=3[C:10]([CH3:20])([CH3:21])[C:11]=2[CH:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6395Methanesulfonic AcidHCID 14798Sodium HydroxideHCID 66835207HCID 66835207, 화합물

생성물 1

HCID 66835135HCID 66835135, 화합물수율 43.4%

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온도
110 °C

실험 절차

Mixture of 3-(3-hydroxy-pyridin-4-yl)-7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound GT15-9, 270 mg) and methanesulfonic acid (1 ml) was stirred and heated at 110° C. for 0.5 hrs. After cooling, the reaction mixture was neutralized with 2 N aqueous solution of sodium hydroxide. The resulting mixture was extracted with the mixture of DCM and MeOH (DCM:MeOH=9:1). The organic layer was concentrated under reduced pressure, and the resulting residues were purified by silica gel column (DCM/MeOH) to obtain the title compound (110 mg, 43%).

후처리

  1. temperatureAfter cooling
  2. extractionThe resulting mixture was extracted with the mixture of DCM and MeOH (DCM:MeOH=9:1)
  3. concentrationThe organic layer was concentrated under reduced pressure
  4. customthe resulting residues were purified by silica gel column (DCM/MeOH)

출처 및 근거

ORD 기록
ord-06c39fc6466246fabfbba8abf322dfbd
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09126931B2

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