HCID 19968441, 화합물 → HCID 11779419, 화합물

HRID 975829노트

반응식

HRID 975829 반응식
S(O)(O)(=O)=O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1>[OH-].[Na+]>[ClH:6].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1

참가 물질

3

반응물 1

HCID 19968441HCID 19968441, 화합물

생성물 1

HCID 11779419HCID 11779419, 화합물

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

A suspension of 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene sulphate (13 g prepared in a similar manner to that described in Example 5) in 1M aqueous sodium hydroxide solution (200 ml) was stirred at ambient temperature for 1 hour, then the free base was extracted into ether (3×150 ml). The extracts were combined, dried over magnesium sulphate, concentrated to a volume of 150 ml, and filtered. The filtrate was cooled in ice and saturated with hydrogen chloride. The resulting solid was collected by filtration, washed with ether, and dried in vacuo at ambient temperature for 24 hours and at 60° C. for 8 hours to give 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene hydrochloride as a white solid. Yield 8.6 g, mp >300° C.

후처리

  1. customprepared in a similar manner to that
  2. extractionthe free base was extracted into ether (3×150 ml)
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated to a volume of 150 ml
  5. filtrationfiltered
  6. temperatureThe filtrate was cooled in ice and saturated with hydrogen chloride
  7. filtrationThe resulting solid was collected by filtration
  8. washwashed with ether
  9. customdried in vacuo at ambient temperature for 24 hours and at 60° C. for 8 hours

출처 및 근거

ORD 기록
ord-de1eb73209b64ad9adec0142c9690f70
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05610161

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