Piperazine → HCID 22291691、化合物

HRID 968117ノート

反応式

HRID 968117 の反応式
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

参加物

4

反応物 2

HCID 4837PiperazineHCID 22291629HCID 22291629、化合物

生成物 1

HCID 22291691HCID 22291691、化合物収率 53%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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

後処理

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

出典と根拠

ORDレコード
ord-2a62aa1f4a654ac78dc3d95a70397d73
出典データセット
uspto-grants-2005_10
特許番号
US06956052B2

反応ノート

読み込み中…