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单水氢氧化锂 → HCID 9935937,化合物

HRID 1069480
笔记
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反应方程式

HRID 1069480 反应方程式
C[O:2][C:3]([C:5]1[N:6]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[C:33]([F:36])([F:35])[F:34])[S:7](=[O:26])(=[O:25])[C:8]2[CH:24]=[CH:23][CH:22]=[CH:21][C:9]=2[C:10]=1[C:11]1[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[C:13]([O:19][CH3:20])[CH:12]=1)=[O:4].O.[OH-].[Li+]>CO.O>[CH3:18][O:17][C:15]1[CH:16]=[C:11]([C:10]2[C:9]3[CH:21]=[CH:22][CH:23]=[CH:24][C:8]=3[S:7](=[O:26])(=[O:25])[N:6]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3[C:33]([F:36])([F:34])[F:35])[C:5]=2[C:3]([OH:4])=[O:2])[CH:12]=[C:13]([O:19][CH3:20])[CH:14]=1
参与物实验过程后处理来源与证据反应笔记

参与物

5

反应物 2

HCID 168937单水氢氧化锂HCID 15512895HCID 15512895,化合物

产物 1

HCID 9935937HCID 9935937,化合物收率 66%

试剂、催化剂与溶剂 2

HCID 887Methanol溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

The solution of 4-(3,5-dimethoxy-phenyl)-2-(2-trifluoromethyl-phenyl)-1,1-dioxo-1,2-dihydro-1λ6-benzo[e][1,2]thiazine-3-carboxylic acid methyl ester (1.29 g, 2.5 mmol) and lithium hydroxide monohydrate (0.3 g 12.5 mmol) in 30 mL of MeOH and 15 mL water was refluxed for 2.5 hours and evaporated to an oil. The residue was dissolved in water, washed with ethyl ether, and the aqueous layer decanted. The aqueous layer was acidified to pH 1 with concentrated HCl and extracted into ethyl ether, washed with brine, dried over anhydrous magnesium sulfate, filtered, and evaporated to a foam. The residue was chromatographed on 50 g silica gel eluted with chloroform, and the appropriate fractions were concentrated in vacuo and evaporated from ethyl ether giving a solid foam, 1.4 g, 66% yield. NMR spectra and elemental analysis were consistent with the structure.

后处理

  1. customevaporated to an oil
  2. dissolutionThe residue was dissolved in water
  3. washwashed with ethyl ether
  4. customthe aqueous layer decanted
  5. extractionextracted into ethyl ether
  6. washwashed with brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customevaporated to a foam
  10. customThe residue was chromatographed on 50 g silica gel
  11. washeluted with chloroform
  12. concentrationthe appropriate fractions were concentrated in vacuo
  13. customevaporated from ethyl ether giving a solid foam, 1.4 g, 66% yield

来源与证据

ORD记录
ord-12bd62d8c2c64cb080bc08a41018549a
来源数据集
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
专利号
US06252070B1

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记