反応式
CCN(C(C)C)C(C)C.[CH2:10]([O:17][C:18]1[CH:32]=[CH:31][C:21]([C:22]([NH:24][C:25]([CH3:30])([CH3:29])[C:26]([OH:28])=O)=[O:23])=[CH:20][CH:19]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.[N:55]1([C:61]([C:63]2[CH:68]=[CH:67][CH:66]=[CH:65][C:64]=2[C:69]([F:72])([F:71])[F:70])=[O:62])[CH2:60][CH2:59][NH:58][CH2:57][CH2:56]1>CN(C=O)C.O>[CH2:10]([O:17][C:18]1[CH:19]=[CH:20][C:21]([C:22]([NH:24][C:25]([CH3:30])([CH3:29])[C:26](=[O:28])[N:58]2[CH2:59][CH2:60][N:55]([C:61](=[O:62])[C:63]3[CH:68]=[CH:67][CH:66]=[CH:65][C:64]=3[C:69]([F:72])([F:70])[F:71])[CH2:56][CH2:57]2)=[O:23])=[CH:31][CH:32]=1)[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1参加物
反応物 5
生成物 1
試薬・触媒・溶媒 2
実験手順
DIPEA (284 mg, 0.19 mL, 1.62 mmol) was added to a stirred solution of 2-(4-benzyloxy-benzoylamino)-2-methyl-propionic acid (170 mg, 0.54 mmol) in DMF (2 mL). HOBT (88 mg, 0.65 mmol) and EDCI (125 mg, 0.65 mmol) were then added at room temperature. After 2 minutes, piperazin-1-yl-(2-trifluoromethyl-phenyl)-methanone hydrochloride salt (192 mg, 0.65 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added and filtered the solid precipitated out to afford 150 mg (50% yield) of 4-benzyloxy-N-{1,1-dimethyl-2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-benzamide. LCMS Purity: 93.29%. 1H NMR (DMSO-d6): δ 8.4 (bs, 1H), 7.6-7.8 (m, 5H), 7.4 (m, 6H), 7.0-7.1 (d, 2H), 5.2 (m, 2H), 3.5 (m, 5H), 3.0 (m, 3H), 1.4 (s, 6H).
後処理
- filtrationfiltered the solid
- customprecipitated out
出典と根拠
- ORDレコード
- ord-70f54ed9e03b4e659104debb51e72d80
- 出典データセット
- uspto-grants-2010_11
- 特許番号
- US07842696B2
関連ノート
読み込み中…