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Hydrochloric Acid → HCID 68643997、化合物

HRID 2388703
ノート
印刷プレビュー

反応式

HRID 2388703 の反応式
Cl.C([N:5]1[CH2:10][CH2:9][C:8]2(N3CCCC3)[O:11][N:12]=[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:7]2[CH:6]1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)(=O)C>>[C:24]1([CH:6]2[C:7]3[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[N:12][O:11][C:8]=3[CH2:9][CH2:10][NH:5]2)[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 68643979HCID 68643979、化合物

生成物 1

HCID 68643997HCID 68643997、化合物収率 50%

反応条件

温度
130 °C

実験手順

Conc. HCl (12 ml) was added to ethyl 5-acetyl-4-phenyl-7a-(pyrrolidin-1-yl)-3a,4,5,6,7,7a-hexahydroisoxazolo[4,5-c]pyridine-3-carboxylate (2 g) at 0° C., and the reaction mixture was heated to 130° C. for 5 h. The hydrochloric acid was evaporated under reduced pressure and the residue was dissolved in dichloromethane and basified with sodium carbonate solution. The organic layer was separated and the aqueous layer was extracted with dichloromethane. The combined organic layers were washed with brine solution and dried over sodium sulfate. The solvent was evaporated under reduced pressure to give the crude compound which was used in the next step without further purification. Yield: 50%.

後処理

  1. customThe hydrochloric acid was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in dichloromethane
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with dichloromethane
  5. washThe combined organic layers were washed with brine solution
  6. dry with materialdried over sodium sulfate
  7. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-3bfc85d0a6ef4d5da6a9f878f7aee0a4
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268814B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート