HCID 19968421, 화합물 → HCID 10220867, 화합물

HRID 975839노트

반응식

HRID 975839 반응식
[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

참가 물질

3

반응물 1

HCID 19968421HCID 19968421, 화합물

생성물 1

HCID 10220867HCID 10220867, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-687324b03dc347b385df4516606728b1
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05610161

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