Hydrochloric Acid → HCID 11779419、化合物

HRID 975840ノート

反応式

HRID 975840 の反応式
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:14]3([CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)[NH:13][CH2:12][CH2:11][CH:10]=2)=[CH:5][CH:4]=1>CCOCC.ClCCl>[ClH:2].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:14]3([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]3)[NH:13][CH2:12][CH2:11][CH:10]=2)=[CH:5][CH:4]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 10220867HCID 10220867、化合物2 回

生成物 1

HCID 11779419HCID 11779419、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

5M Hydrochloric acid (200 ml) was added slowly to a solution of 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene (98 g) in ether (1 l) and the mixture was stirred at ambient temperature for 30 minutes. The resulting solid was collected by filtration and washed with cold water followed by dichloromethane to give an off-white solid. The process was repeated using the remainder of 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene to give further off-white solid. The combined solids were stirred in dichloromethane (1 l) for 1 hour, collected by filtration, washed with dichloromethane (200 ml) and dried in vacuo to give 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene hydrochloride as an off-white solid. Yield 224.3 g, mp >300° C.

後処理

  1. filtrationThe resulting solid was collected by filtration
  2. washwashed with cold water
  3. customto give an off-white solid
  4. customto give further off-white solid
  5. filtrationcollected by filtration
  6. washwashed with dichloromethane (200 ml)
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-a9047464546946a8a72f91be8ae4c986
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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