Water → Agn-PC-0MW2M5

HRID 1635936ノート

反応式

HRID 1635936 の反応式
S([CH2:11][N+:12]#[C-:13])(C1C=CC(C)=CC=1)(=O)=O.[CH3:14][C:15]([CH3:18])([O-])[CH3:16].[K+].O.[CH2:21]([O:23][C:24](=[O:26])[CH3:25])[CH3:22].[CH3:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32].O1CCC[CH2:34]1>>[C:15]1([C:18]2[C:25]([C:24]([O:23][CH2:21][CH3:22])=[O:26])=[CH:11][NH:12][CH:13]=2)[C:16]2[C:29](=[CH:30][CH:31]=[CH:32][CH:34]=2)[CH:28]=[CH:27][CH:14]=1

参加物

6

反応物 5

HCID 962WaterHCID 8028Tetrahydrofuran2 回HCID 161915Tosylmethyl isocyanideHCID 21226206Ethyl acetate hexaneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 9943237Agn-PC-0MW2M5収率 77%

実験手順

5 g(18.9 mmol) of the compound prepared in Preparation 1-1) and 3.68 g(18.9 mmol) of tosylmethylisocyanide were dissolved in 100 ml of tetrahydrofuran. 2.55 g(22.7 mmol) of potassium t-butoxide dissolved in 100 ml of tetrahydrofuran was slowly added thereto and the resulting mixture was refluxed for 30 minutes. 100 ml of water was added to the reaction solution to stop the reaction and the solvent was removed under reduced pressure. The residue was extracted with diethylether, washed with saturated sodium chloride solution and dried over magnesium sulfate. Then, the solvent was removed under reduced pressure and the residue was subjected to column chromatography(eluent: ethylacetate/n-hexane=⅓, v/v) to give 3.85 g(14.5 mmol, Yield 77%) of the title compound.

後処理

  1. additionwas slowly added
  2. temperaturethe resulting mixture was refluxed for 30 minutes
  3. customthe reaction
  4. customthe solvent was removed under reduced pressure
  5. extractionThe residue was extracted with diethylether
  6. washwashed with saturated sodium chloride solution
  7. dry with materialdried over magnesium sulfate
  8. customThen, the solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-248ccb57a903429fb3282073a2927f72
出典データセット
uspto-grants-2003_01
特許番号
US06511978B1

反応ノート

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