HCID 19968441、化合物 → HCID 11779419、化合物

HRID 975829ノート

反応式

HRID 975829 の反応式
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

参加物

3

反応物 1

HCID 19968441HCID 19968441、化合物

生成物 1

HCID 11779419HCID 11779419、化合物

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-de1eb73209b64ad9adec0142c9690f70
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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