反応式
[O:1]=[C:2]1[C:6]2[N:7]=[N:8][C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=3[C:5]=2[NH:4][N:3]1[C:15]1[CH:23]=[CH:22][C:18]([C:19](Cl)=[O:20])=[CH:17][CH:16]=1.C(N(C(C)C)CC)(C)C.[CH:33]1([NH:39][CH2:40][CH2:41][CH2:42][NH2:43])[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]1.O>CC(N(C)C)=O>[CH:33]1([NH:39][CH2:40][CH2:41][CH2:42][NH:43][C:19](=[O:20])[C:18]2[CH:22]=[CH:23][C:15]([N:3]3[C:2](=[O:1])[C:6]4[N:7]=[N:8][C:9]5[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=5[C:5]=4[NH:4]3)=[CH:16][CH:17]=2)[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
4-(3-oxo-1,3-dihydro-2H-pyrazolo[4,3-c]cinnolin-2-yl)benzoyl chloride (97 mg, 0.30 mmol) was dissolved in anhydrous DMA (2 ml). Diisopropylethylamine (39 mg, 53 μl, 0.60 mmol) was added followed by N-cyclohexyl-1,3-propanediamine (52 mg, 0.60 mmol). The mixture was stirred for 30 min. Water (5 ml) was added to give a dark red suspension. The mixture was extracted with n-butanol (2×20 ml). The combined organic phases were washed with water and concentrated under vacuum until precipitation was observed. Hexane (20 ml) and ethyl acetate (10 ml) were added, the solids were collected by filtration and dried under vacuum. The product was isolated as a dark red powder (82 mg, 0.18 mmol, 62%). LCMS: m/z 445 [M+H]+.
後処理
- customto give a dark red suspension
- extractionThe mixture was extracted with n-butanol (2×20 ml)
- washThe combined organic phases were washed with water
- concentrationconcentrated under vacuum until precipitation
- additionHexane (20 ml) and ethyl acetate (10 ml) were added
- filtrationthe solids were collected by filtration
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-77cb856243b14e27b9debc2173a52b28
- 出典データセット
- uspto-grants-2009_10
- 特許番号
- US07598247B2
関連ノート
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