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Trifluoroacetic acid → HCID 71618475、化合物

HRID 64469
ノート
印刷プレビュー

反応式

HRID 64469 の反応式
[CH:1]1([CH2:7][O:8][C:9]2[C:10]3[N:11]([C:15]([C:19]([NH:21][C@H:22]([CH2:31][CH:32]([CH3:34])[CH3:33])[CH2:23][C:24]([O:26]C(C)(C)C)=[O:25])=[O:20])=[C:16]([CH3:18])[N:17]=3)[CH:12]=[CH:13][CH:14]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.FC(F)(F)C(O)=O>ClCCl>[CH:1]1([CH2:7][O:8][C:9]2[C:10]3[N:11]([C:15]([C:19]([NH:21][C@H:22]([CH2:31][CH:32]([CH3:34])[CH3:33])[CH2:23][C:24]([OH:26])=[O:25])=[O:20])=[C:16]([CH3:18])[N:17]=3)[CH:12]=[CH:13][CH:14]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 86713494tert-butyl (3R)-3-({[8-(cyclohexylmethoxy)-2-methylimidazo[1,2-a]pyridin-3-yl]carbonyl}amino)-5-methylhexanoate

生成物 1

HCID 71618475HCID 71618475、化合物収率 77.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 216 mg of tert-butyl (3R)-3-({[8-(cyclohexylmethoxy)-2-methylimidazo[1,2-a]pyridin-3-yl]carbonyl}amino)-5-methylhexanoate in 2 ml of dichloromethane was added 2 ml of trifluoroacetic acid, followed by stirring overnight. The solvent was evaporated under reduced pressure, and water, a saturated aqueous sodium hydrogen carbonate solution, 1 M hydrochloric acid, and chloroform were added thereto to carry out a layer separation operation. The organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography. To the obtained purified product were added ethyl acetate and diisopropyl ether, and the resulting solid was collected by filtration and dried to obtain 147 mg of (3R)-3-({[8-(cyclohexylmethoxy)-2-methylimidazo[1,2-a]pyridin-3-yl]carbonyl}amino)-5-methylhexanoic acid.

後処理

  1. customThe solvent was evaporated under reduced pressure, and water
  2. additiona saturated aqueous sodium hydrogen carbonate solution, 1 M hydrochloric acid, and chloroform were added
  3. customa layer separation operation
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customthe obtained residue was purified by silica gel column chromatography
  7. customTo the obtained purified product
  8. additionwere added ethyl acetate and diisopropyl ether
  9. filtrationthe resulting solid was collected by filtration
  10. customdried

出典と根拠

ORDレコード
ord-c7043a3f44dc44949fc3181cf001c9be
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09447090B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート