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1,2-Dimethoxyethane → HCID 66975737、化合物

HRID 1022686
ノート
印刷プレビュー

反応式

HRID 1022686 の反応式
[NH2:1][CH2:2][C@H:3]1[C@H:9]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([Cl:17])[CH:11]=2)[O:8][CH2:7][CH2:6][N:5]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:4]1.[OH-].[Na+].[CH2:27]([CH2:30][O:31]C)[O:28]C>>[Cl:17][C:12]1[CH:11]=[C:10]([C@@H:9]2[O:8][CH2:7][CH2:6][N:5]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:4][C@H:3]2[CH2:2][NH:1][C:27](=[O:28])[CH2:30][OH:31])[CH:15]=[CH:14][C:13]=1[Cl:16]
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 3

HCID 80711,2-DimethoxyethaneHCID 14798Sodium HydroxideHCID 66975351HCID 66975351、化合物

生成物 1

HCID 66975737HCID 66975737、化合物

実験手順

To a solution of tert-butyl (6R,7R)-6-(aminomethyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (171 mg) in dimethoxyethane (3 mL) was added 1 N aqueous sodium hydroxide solution (0.72 ml), and the mixture was stirred overnight. The solvent was evaporated under reduced pressure. Water was added to the residue, and the mixture was extracted twice with ethyl acetate. The combined organic layers were washed with brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate/hexane) to give the title compound (157 mg).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. additionWater was added to the residue
  3. extractionthe mixture was extracted twice with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-e52affe2c7af45669537936cdc042f03
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722662B2

反応ノート

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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