Biphenyl-4-sulfonic acid [2-(tert-butyl-diphenyl-silanyloxy)-ethyl]-(4-hydroxy-butyl)-amide → Biphenyl-4-sulfonic acid-(4-hydroxybutyl)-(2-hydroxyethyl)-amide

HRID 2425125ノート

反応式

HRID 2425125 の反応式
C([Si](C1C=CC=CC=1)(C1C=CC=CC=1)[O:6][CH2:7][CH2:8][N:9]([CH2:25][CH2:26][CH2:27][CH2:28][OH:29])[S:10]([C:13]1[CH:18]=[CH:17][C:16]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:15][CH:14]=1)(=[O:12])=[O:11])(C)(C)C>[F-].C([NH3+])(C)(C)C>[OH:29][CH2:28][CH2:27][CH2:26][CH2:25][N:9]([CH2:8][CH2:7][OH:6])[S:10]([C:13]1[CH:18]=[CH:17][C:16]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:15][CH:14]=1)(=[O:12])=[O:11]

参加物

3

反応物 1

HCID 59728311Biphenyl-4-sulfonic acid [2-(tert-butyl-diphenyl-silanyloxy)-ethyl]-(4-hydroxy-butyl)-amide

生成物 1

HCID 11624455Biphenyl-4-sulfonic acid-(4-hydroxybutyl)-(2-hydroxyethyl)-amide

試薬・触媒・溶媒 1

HCID 21866379t-Butylammonium fluoride溶媒

実験手順

Biphenyl-4-sulfonic acid [2-(tert-butyl-diphenyl-silanyloxy)-ethyl]-(4-hydroxy-butyl)-amide (1 g) was dissolved in tertiarybutylammonium fluoride (15 mL of 1 M in tetrahydrafuran) and stirring for 30 minutes. The solvent was evaporated and the residue dissolved in methylene chloride, washed with water and dried over Na2SO4. The product was purified by column chromatography (ethyl acetate: light petroleum) to give the title compound. δC (DMSO, 62.9 MHz): 25.1, 29.5, 48.9, 51.2, 57.9, 60.3, 127.1, 127.2, 127.6, 128.6, 129.2, 138.1, 138.4 and 144.1.

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe residue dissolved in methylene chloride
  3. washwashed with water
  4. dry with materialdried over Na2SO4
  5. customThe product was purified by column chromatography (ethyl acetate: light petroleum)

出典と根拠

ORDレコード
ord-2d3df3ca72e440068f81e2ec50b61f5b
出典データセット
uspto-grants-2011_06
特許番号
US07964643B2

反応ノート

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