Trimethylsilyl iodide → {2-[(4'-Octyloxy-biphenyl-4-carbonyl)-amino]-benzyl}-phosphonic acid

HRID 1642063ノート

反応式

HRID 1642063 の反応式
C([O:3][P:4]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[NH:16][C:17]([C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:30]=[CH:29][C:28]([O:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])=[CH:27][CH:26]=2)=[CH:21][CH:20]=1)=[O:18])(=[O:8])[O:5]CC)C.C[Si](I)(C)C>C(Cl)Cl.C1(C)C=CC=CC=1.[OH-].[Na+]>[CH2:32]([O:31][C:28]1[CH:27]=[CH:26][C:25]([C:22]2[CH:23]=[CH:24][C:19]([C:17]([NH:16][C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[CH2:9][P:4](=[O:3])([OH:8])[OH:5])=[O:18])=[CH:20][CH:21]=2)=[CH:30][CH:29]=1)[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39]

参加物

6

反応物 2

HCID 85247Trimethylsilyl iodideHCID 86638333{2-[(4'-Octyloxy-biphenyl-4-carbonyl)-amino]-benzyl}-phosphonic acid diethylester

生成物 1

HCID 24824095{2-[(4'-Octyloxy-biphenyl-4-carbonyl)-amino]-benzyl}-phosphonic acid

試薬・触媒・溶媒 3

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

{2-[(4′-Octyloxy-biphenyl-4-carbonyl)-amino]-benzyl}-phosphonic acid diethylester is dissolved in CH2Cl2 and and the mixture obtained is treated with trimethylsilyl iodide at 0°. The mixture obtained is stirred at 0° for several hours and diluted with toluene. From the mixture obtained solvent is evaporated. The evaporation residue obtained is dissolved in 1N NaOH solution, washed with EtOAc, HCl is added, precipitation occurs and the precipitate obtained is collected. {2-[(4′-Octyloxy-biphenyl-4-carbonyl)-amino]-benzyl}-phosphonic acid is obtained.

後処理

  1. customthe mixture obtained
  2. customThe mixture obtained
  3. customFrom the mixture obtained solvent
  4. customis evaporated
  5. customThe evaporation residue obtained
  6. washwashed with EtOAc, HCl
  7. additionis added
  8. customprecipitation
  9. customthe precipitate obtained
  10. customis collected

出典と根拠

ORDレコード
ord-f5e0ed5eecc64310a2d55969935066ad
出典データセット
uspto-grants-2012_02
特許番号
US08119617B2

反応ノート

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