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甲基磺酸 → HCID 66835135,化合物

HRID 61908
笔记
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反应方程式

HRID 61908 反应方程式
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
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

4

反应物 3

HCID 6395甲基磺酸HCID 14798氢氧化钠HCID 66835207HCID 66835207,化合物

产物 1

HCID 66835135HCID 66835135,化合物收率 43.4%

反应条件

温度
110 °C

实验过程

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%).

后处理

  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)

来源与证据

ORD记录
ord-1cff5ac194c84d2d9c7ba131a54a0b7d
来源数据集
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
专利号
US09440922B2

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记