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Hydrochloric Acid → HCID 13799019、化合物

HRID 255880
ノート
印刷プレビュー

反応式

HRID 255880 の反応式
Cl[CH:2]1[C:10]2[C:5](=[C:6]([O:11][CH3:12])[CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3]1.[NH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1.Cl>C(Cl)(Cl)Cl>[CH3:12][O:11][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[CH2:4][CH2:3][CH:2]2[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 8082PiperidineHCID 13799018HCID 13799018、化合物

生成物 1

HCID 13799019HCID 13799019、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

A solution of 1-chloro-4-methoxyindan (from Step 3) in chloroform (130 ml) is added over a period of ten minutes to a stirred mixture of piperidine (284 ml) in chloroform (400 ml) under nitrogen. The reaction mixture is heated to reflux for six hours and allowed to stand at RT overnight. The mixture is treated with 10% aqueous HCl and the organic layer separated. The aqueous layer is extracted with methylene chloride and the combined organic extracts washed with 10% aqueous HCl. The organic layer is evaporated in vacuo and the residue partitioned between 5% aqueous HCl and ether. The combined aqueous fraction is washed with ether, made alkaline, and the alkaline layer extracted with ether. The ether extract is washed, dried and concentrated in vacuo yielding the piperidine indan as an oil.

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux for six hours
  3. customthe organic layer separated
  4. extractionThe aqueous layer is extracted with methylene chloride
  5. washthe combined organic extracts washed with 10% aqueous HCl
  6. customThe organic layer is evaporated in vacuo
  7. customthe residue partitioned between 5% aqueous HCl and ether
  8. washThe combined aqueous fraction is washed with ether
  9. extractionthe alkaline layer extracted with ether
  10. extractionThe ether extract
  11. washis washed
  12. customdried
  13. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-d7454a20d96343bfb90046ef3ef9afa8
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04699906

反応ノート

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