Hydrochloric Acid → HCID 11779419, 화합물

HRID 975840노트

반응식

HRID 975840 반응식
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

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 10220867HCID 10220867, 화합물2회

생성물 1

HCID 11779419HCID 11779419, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a9047464546946a8a72f91be8ae4c986
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05610161

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