反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[N:11]=[C:12]([NH:15][C:16](=[O:34])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23]([NH:25][O:26]CC2C=CC=CC=2)=[O:24])[S:13][CH:14]=1)([O-:3])=[O:2].B(Br)(Br)Br>C(Cl)Cl>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[N:11]=[C:12]([NH:15][C:16](=[O:34])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23]([NH:25][OH:26])=[O:24])[S:13][CH:14]=1)([O-:3])=[O:2]参加物
4
実験手順
A mixture of compound 15 (0.040 g, 0.083 mmol) in methylene chloride (1 mL) was cooled to −30° C. while boron tribromide (0.18 ml) 1M in methylene chloride was added dropwise. After stirring at room temperature for 2 hours, the mixture was cooled to 0° C. and quenched with saturated sodium bicarbonate. The reaction mixture was diluted with ethyl acetate and washed sequentially with saturated NaHCO3, and brine. The organic layer was dried over sodium sulfate and concentrated in vacuo to provide a crude residue which was purified by reverse phase HPLC to afford octanedioic acid hydroxyamide [4-(2-nitro-phenyl)-thiazol-2-yl]-amide 17 (0.018 g, 55% yield).
後処理
- additionwas added dropwise
- temperaturethe mixture was cooled to 0° C.
- customquenched with saturated sodium bicarbonate
- additionThe reaction mixture was diluted with ethyl acetate
- washwashed sequentially with saturated NaHCO3, and brine
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated in vacuo
- customto provide a crude residue which
- customwas purified by reverse phase HPLC
出典と根拠
- ORDレコード
- ord-8a1e2a1969604e45b6608a012916bb36
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653278B2
関連ノート
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