Piperazine → HCID 22291691, 화합물

HRID 457321노트

반응식

HRID 457321 반응식
Cl[C:2]1[CH:3]=[C:4]([C:31]([Cl:34])=[CH:32][N:33]=1)[C:5]([NH:7][C:8]1[CH:30]=[CH:29][C:11]2[CH2:12][CH2:13][C:14]3[C:15]([C:26]([NH2:28])=[O:27])=[N:16][N:17]([C:19]4[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=4)[C:18]=3[C:10]=2[CH:9]=1)=[O:6].[NH:35]1[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]1>CCO>[Cl:34][C:31]1[C:4]([C:5]([NH:7][C:8]2[CH:30]=[CH:29][C:11]3[CH2:12][CH2:13][C:14]4[C:15]([C:26]([NH2:28])=[O:27])=[N:16][N:17]([C:19]5[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=5)[C:18]=4[C:10]=3[CH:9]=2)=[O:6])=[CH:3][C:2]([N:35]2[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]2)=[N:33][CH:32]=1

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 22291629HCID 22291629, 화합물

생성물 1

HCID 22291691HCID 22291691, 화합물수율 53%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The title compound was synthesized by the same procedure as in Example 214 starting with the title compound of Example 248 (1 g, 0.0020 mol) and piperazine (3.44 g, 0.040 mol) in 5 mL of EtOH. The reaction was run at 100° C. for 24 h. The off-white precipitate that formed in the crude reaction mixture was filtered and washed with EtOH to afford 0.579 g of title compound (yield: 53%). 1H NMR (300 MHz, d6-DMSO): 2.67 (t, 4H, J=4.9 Hz), 2.85–2.90 (m, 4H), 3.36 (t, 4H, J=4.9 Hz), 6.80 (s, 1H), 7.18–7.19 (m, 1H), 7.25 (s, 1H), 7.27–7.35 (m, 3H), 7.37–7.39 (dd, 1H, J=8 Hz, 2 Hz), 7.51–7.55 (m, 3H), 8.09 (s, 1H), 10.28 (s, 1H). M=1=547

후처리

  1. customThe off-white precipitate that formed in the crude
  2. customreaction mixture
  3. filtrationwas filtered
  4. washwashed with EtOH

출처 및 근거

ORD 기록
ord-16774b9e48d9471bbf6e4bf189b72742
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07186743B2

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