反応式
Cl.[CH3:2][NH:3][O:4][CH3:5].[CH3:6][N:7]1[C:11]([C:12]([OH:14])=O)=[CH:10][CH:9]=[N:8]1.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.C(N(C(C)C)CC)(C)C>O.CN(C)C=O>[CH3:5][O:4][N:3]([CH3:2])[C:12]([C:11]1[N:7]([CH3:6])[N:8]=[CH:9][CH:10]=1)=[O:14]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
N,O-dimethylhydroxylamine hydrochloride (1.30 g) was added to an dimethylformamide (32 mL) solution that contained 1-methyl-1H-pyrazol-5-carboxylic acid (1.21 g), O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (4.38 g) and diisopropylethylamine (3.34 mL) at a room temperature, and the obtained solution was then stirred for 2 hours. Thereafter, water was added to the reaction solution, and the obtained mixture was then extracted with ethyl acetate. The organic layer was washed with water and a saturated saline, and was then dried over anhydrous magnesium sulfate, followed by vacuum concentration. The residue was purified by column chromatography (silica gel cartridge, chloroform:methanol=100:0 to 95:5), so as to obtain the title compound (1.03 g) in the form of a yellow oily substance.
後処理
- customat a room temperature
- extractionthe obtained mixture was then extracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materiala saturated saline, and was then dried over anhydrous magnesium sulfate
- concentrationfollowed by vacuum concentration
- customThe residue was purified by column chromatography (silica gel cartridge, chloroform:methanol=100:0 to 95:5)
出典と根拠
- ORDレコード
- ord-01aaea0725f54f8e882d584f78333ee0
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08642626B2
関連ノート
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