HCID 19968421、化合物 → HCID 10220867、化合物

HRID 975839ノート

反応式

HRID 975839 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2(O)[C:13]3([CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]3)[NH:12][CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]3([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18]3)[NH:12][CH2:11][CH2:10][CH:9]=2)=[CH:4][CH:3]=1

参加物

3

反応物 1

HCID 19968421HCID 19968421、化合物

生成物 1

HCID 10220867HCID 10220867、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

5-(4-Chlorophenyl)-5-hydroxy-1-azaspiro[5.5]undecane (105.1 g) was added in portions to vigorously stirred concentrated sulphuric acid (600 ml) over 20 minutes, then the mixture was stirred at ambient temperature for a further 1 hour and poured carefully onto ice (2 l) causing a white solid to precipitate. The mixture was cooled in ice for 2 hours and the solid was collected by filtration. The solid was basified by addition to an excess of 5M aqueous sodium hydroxide solution and the product was extracted into ether (4×200 ml) followed by dichloromethane (2×250 ml). The extracts were combined, dried over sodium sulphate and the solvents removed in vacuo to give 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene as a cream solid. Yield 98 g.

後処理

  1. additionpoured carefully onto ice (2 l)
  2. customto precipitate
  3. temperatureThe mixture was cooled in ice for 2 hours
  4. filtrationthe solid was collected by filtration
  5. additionThe solid was basified by addition to an excess of 5M aqueous sodium hydroxide solution
  6. extractionthe product was extracted into ether (4×200 ml)
  7. dry with materialdried over sodium sulphate
  8. customthe solvents removed in vacuo

出典と根拠

ORDレコード
ord-687324b03dc347b385df4516606728b1
出典データセット
uspto-grants-1997_03
特許番号
US05610161

反応ノート

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