反応式
[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[CH:4][C:3]=1[C:8]([OH:10])=O.[NH2:11][CH2:12][CH2:13][NH:14][C:15]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(N(CC)CC)C.Cl.CN(C)CCCN=C=NCC>C(Cl)(Cl)Cl>[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[CH:4][C:3]=1[C:8]([NH:11][CH2:12][CH2:13][NH:14][C:15]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:10]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 5-amino-1-methyl-1H-pyrazole-4-carboxylic acid (7.1 g), N-(2-aminoethyl)tritylamine (15.1 g) and triethylamine (10.1 g) in chloroform (200 ml) was added N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (9.6 g), and the mixture was stirred at room temperature for 16 hours. The reaction mixture was washed successively with 10% aqueous citric acid solution, brine and saturated aqueous sodium hydrogencarbonate solution. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue was triturated with ethyl acetate and dried in vacuo to give 5-amino-1-methyl-N-[2-(tritylamino)ethyl]-1H-pyrazole-4-carboxamide (11.4 g) as a solid.
後処理
- washThe reaction mixture was washed successively with 10% aqueous citric acid solution, brine and saturated aqueous sodium hydrogencarbonate solution
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was triturated with ethyl acetate
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-812a5b8ee45345569b5df881917c8b58
- 出典データセット
- uspto-grants-2007_03
- 特許番号
- US07192943B2
関連ノート
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