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Hydrogen chloride-ethyl acetate → HCID 68935247、化合物

HRID 1260926
ノート
印刷プレビュー

反応式

HRID 1260926 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]2[C@H:14]([N:15]([CH3:24])[C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[O:17])[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].Cl.C(OCC)(=O)C>C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]2[C@H:14]([N:15]([CH3:24])[C:16](=[O:17])[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:13][CH2:12][NH:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]
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 86631305rel-1,1-Dimethylethyl (3R,4R)-4-(benzoylmethylamino)-3-(3,4-dichlorophenyl)-1-piperidinecarboxylate

生成物 1

HCID 68935247HCID 68935247、化合物収率 75.7%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of the compound (0.455 g) obtained in Example 13 in ethyl acetate (3 mL) was added 4N hydrogen chloride/ethyl acetate solution (3 mL), and the mixture was stirred at room temperature for 24 hr with heating. The reaction mixture was concentrated under reduced pressure, ethyl acetate was added to the residue, and the mixture was made basic with 2N aqueous sodium hydroxide solution. The organic layer was separated, washed with water, and the solvent was evaporated under reduced pressure to give the title compound (0.27 g, 75%) as a white powder.

後処理

  1. temperaturewith heating
  2. concentrationThe reaction mixture was concentrated under reduced pressure, ethyl acetate
  3. additionwas added to the residue
  4. customThe organic layer was separated
  5. washwashed with water
  6. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-0349a66488aa48f59f90d58cab307f0c
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08470816B2

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