Potassium Carbonate → HCID 11327149, 화합물

HRID 1354061

반응식

HRID 1354061 반응식
Cl.[Cl:2][C:3]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:4]=1[N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:23][CH2:24][C:25]([N:27]1[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH2:29][CH2:28]1)=[O:26]>CC(=O)CC.CN(C)C=O>[Cl:2][C:3]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:4]=1[N:10]1[CH2:15][CH2:14][N:13]([CH2:23][CH2:24][C:25]([N:27]2[C:35]3[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=3)[CH2:29][CH2:28]2)=[O:26])[CH2:12][CH2:11]1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 27948813-chloro-1-(2,3-dihydro-1H-indol-1-yl)propan-1-oneHCID 116303721-(2,3-Dichlorophenyl)piperazine hydrochloride

생성물 1

HCID 11327149HCID 11327149, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6569Methyl Ethyl Ketone용매

반응 조건

온도
50 °C

실험 절차

A mixture of 1-(2,3-dichlorophenyl)piperazine, hydrochloride (8.0 g) and potassium carbonate (15 g) in a mixture of butanone (50 mL) and dimethyl formamide (5 mL) was heated to 50° C. followed by the addition of 3-chloro-1-(2,3-dihydro-1H-indol-1-yl)propan-1-one (6.0 g). The resulting mixture was boiled under reflux for 40 h and filtered hot. The remaining organic phase was left to crystallise, and a white crystalline material was collected by filtration and washed with acetone (8.5 g). Mp 157–158° C. 1H NMR (DMSO-d6): 2.60 (s, 4H); 2.60–2.80 (m, 4H); 3.00 (s, 4H); 3.15 (t, 2H); 4.10 (t, 2H); 6.95 (t, 1H); 7.10–7–15 (m, 2H); 7.20 (d, 1H); 7.25–7.35 (m, 2H); 8.10 (d, 1H). MS m/z: 404 (MH+), 243.

후처리

  1. temperatureunder reflux for 40 h
  2. filtrationfiltered hot
  3. waitThe remaining organic phase was left
  4. customto crystallise
  5. filtrationa white crystalline material was collected by filtration
  6. washwashed with acetone (8.5 g)

출처 및 근거

ORD 기록
ord-bfb870f7493742309f0603d59a5ed023
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07223765B2

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