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Hydrogen chloride-ethyl acetate → tert-butyl (1S,2R)-1-amino-7-methylindane-2-carboxylate

HRID 64428
ノート
印刷プレビュー

反応式

HRID 64428 の反応式
C([S@@]([NH:7][C@@H:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][C:15]=2[CH3:17])[CH2:10][C@H:9]1[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=O)(C)(C)C.Cl.C(OCC)(=O)C>C(OCC)(=O)C>[NH2:7][C@@H:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][C:15]=2[CH3:17])[CH2:10][C@H:9]1[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19]
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 21866389Hydrogen chloride-ethyl acetateHCID 86713440tert-butyl (1S,2R)-1-{[(S)-tert-butylsulfinyl]amino}-7-methylindane-2-carboxylate

生成物 1

HCID 86713439tert-butyl (1S,2R)-1-amino-7-methylindane-2-carboxylate収率 89.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 140 mg of tert-butyl (1S,2R)-1-{[(S)-tert-butylsulfinyl]amino}-7-methylindane-2-carboxylate in 9.1 ml of ethyl acetate was added 0.88 ml of a 4 M hydrogen chloride/ethyl acetate solution, followed by stirring at room temperature for 2 hours. The solvent was evaporated under reduced pressure, and to the obtained residue were added a saturated aqueous sodium hydrogen carbonate solution and ethyl acetate to carry out a layer separation operation. The organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to obtain 88 mg of tert-butyl (1S,2R)-1-amino-7-methylindane-2-carboxylate.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. additionto the obtained residue were added a saturated aqueous sodium hydrogen carbonate solution and ethyl acetate
  3. customa layer separation operation
  4. washThe organic layer was washed with water and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-a622f2db1df140b3965c7e7120b30305
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

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