Trifluoroacetic acid → Methyl (2,3-dioxopiperazin-1-YL)acetate
反応式
COC1C=C(OC)C=CC=1C[N:6]1[CH2:11][CH2:10][N:9]([CH2:12][C:13]([O:15][CH3:16])=[O:14])[C:8](=[O:17])[C:7]1=[O:18].FC(F)(F)C(O)=O.C1(OC)C=CC=CC=1>>[O:17]=[C:8]1[C:7](=[O:18])[NH:6][CH2:11][CH2:10][N:9]1[CH2:12][C:13]([O:15][CH3:16])=[O:14]参加物
4
実験手順
A mixture of 10.5 g of methyl [4-(2,4-dimethoxybenzyl)-2,3-dioxopiperazin-1-yl]acetate, 42 ml of trifluoroacetic acid and 21 ml of anisole was refluxed for 4 hours. The reaction mixture was cooled to room temperature and then distilled under reduced pressure to remove the solvent. The resulting residue was purified by a silica gel column chromatography (eluent; chloroform: methanol=6:1) to obtain 4.5 g of methyl (2,3-dioxopiperazin-1-yl)acetate as colorless crystals.
後処理
- temperaturewas refluxed for 4 hours
- distillationdistilled under reduced pressure
- customto remove the solvent
- customThe resulting residue was purified by a silica gel column chromatography (eluent; chloroform: methanol=6:1)
出典と根拠
- ORDレコード
- ord-5112ee19f9ef4244ac9519c82f054e02
- 出典データセット
- uspto-grants-1999_03
- 特許番号
- US05877174
反応ノート
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