反応式
C(N(C(C)C)CC)(C)C.Cl.[NH2:11][CH2:12][CH2:13][N:14]1[C:19]([C:20]2[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][C:21]=2[O:28][CH3:29])=[CH:18][C:17](=[O:30])[NH:16][C:15]1=[S:31].Cl.[N:33]1([C:38](N)=[NH:39])C=CC=N1>CN(C=O)C.CCO>[CH3:29][O:28][C:21]1[CH:22]=[C:23]([O:26][CH3:27])[CH:24]=[CH:25][C:20]=1[C:19]1[N:14]([CH2:13][CH2:12][N:11]=[C:38]([NH2:39])[NH2:33])[C:15](=[S:31])[NH:16][C:17](=[O:30])[CH:18]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 55 °C
実験手順
Diisopropylethylamine (0.22 mL, 1.3 mmol) was added to a suspension of 1-(2-aminoethyl)-6-(2,4-dimethoxyphenyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one hydrochloride (181.6 mg, 0.528 mmol) (the product of Example 6) and 1H-pyrazole-1-carboxamidine hydrochloride (90.6 mg, 0.618 mmol) in DMF (0.55 mL). After heating for 1 h at 55° C., the reaction mixture was cooled to ambient temperature, diluted with EtOH (1.6 mL), and the solid product collected by vacuum filtration, rinsing with additional EtOH. The isolated solid was re-suspended in EtOH (2.1 mL) for 3 h at r.t. before being collected again by vacuum filtration and rinsing with additional EtOH. The desired product was obtained, after drying, as a colorless solid. Solubility data for this product is consistent with it being in its zwitterionic form.
後処理
- temperaturethe reaction mixture was cooled to ambient temperature
- filtrationthe solid product collected by vacuum filtration
- washrinsing with additional EtOH
- filtrationbefore being collected again by vacuum filtration
- washrinsing with additional EtOH
出典と根拠
- ORDレコード
- ord-557a2456f3b545a5a2527875a72f4977
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09399626B2
関連ノート
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