1-(3-Chlorophenyl)piperazine monohydrochloride → 8-[3-[4-(3-Chlorophenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrate

HRID 868549노트

반응식

HRID 868549 반응식
Br[CH2:2][CH2:3][CH2:4][O:5][N:6]1[C:15](=[O:16])[CH2:14][C:9]2([CH2:13][CH2:12][CH2:11][CH2:10]2)[CH2:8][C:7]1=[O:17].[ClH:18].[Cl:19][C:20]1[CH:21]=[C:22]([N:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)[CH:23]=[CH:24][CH:25]=1>CCN(CC)CC>[OH2:5].[ClH:19].[Cl:19][C:20]1[CH:21]=[C:22]([N:26]2[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][O:5][N:6]3[C:15](=[O:16])[CH2:14][C:9]4([CH2:13][CH2:12][CH2:11][CH2:10]4)[CH2:8][C:7]3=[O:17])[CH2:28][CH2:27]2)[CH:23]=[CH:24][CH:25]=1.[Cl:19][C:20]1[CH:21]=[C:22]([N:26]2[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][O:5][N:6]3[C:15](=[O:16])[CH2:14][C:9]4([CH2:13][CH2:12][CH2:11][CH2:10]4)[CH2:8][C:7]3=[O:17])[CH2:28][CH2:27]2)[CH:23]=[CH:24][CH:25]=1.[ClH:18]

참가 물질

4

반응물 2

HCID 256811-(3-Chlorophenyl)piperazine monohydrochlorideHCID 142805838-(3-Bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione

생성물 1

HCID 1317157328-[3-[4-(3-Chlorophenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrate

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

A solution of 8-(3-bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione (4.0 g) and 1-(3-chlorophenyl)piperazine hydrochloride (3.06 g) in 50 ml of Et3N was heated to reflux with stirring under N2. After 1 hour TLC (thin layer chromatography) showed the absence of starting material. The excess Et3N was removed in vacuo and the residue chromatographed on silica using ethyl acetate as the eluent. Fractions containing the desired product were combined and concentrated in vacuo.

후처리

  1. temperatureto reflux
  2. customThe excess Et3N was removed in vacuo
  3. customthe residue chromatographed on silica
  4. additionFractions containing the desired product
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-1ba4e93a36a248379f4efa5efff7e99b
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04780466

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