反応式
[OH:1][CH2:2][CH:3]([CH2:6][OH:7])[CH2:4][OH:5].[F:8][CH2:9][C:10]([CH2:12][F:13])=O.C(OC)(OC)OC.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(N(CC)CC)C>[F:8][CH2:9][C:10]1([CH2:12][F:13])[O:5][CH2:4][CH:3]([CH2:6][OH:7])[CH2:2][O:1]1参加物
6
反応条件
- 温度
- 60 °C
実験手順
A mixture of 2-(hydroxymethyl)-1,3-propanediol (2.2 g, 20.7 mmol), 1,3-difluoroacetone (3.89 g, 41.4 mmol), trimethyl orthoformate (3.44 ml, 20.7 mmol), and p-toluenesulfonic acid monohydrate (356 mg, 2.07 mmol) was stirred at 60° C. for 10 hours. After completion of the reaction, triethylamine (577 μl) was added to the reaction mixture, which was then concentrated. The residue was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate) to obtain the title compound (1.6 g, yield: 43.4%) as a light yellow oil.
後処理
- additionwas added to the reaction mixture, which
- concentrationwas then concentrated
- customThe residue was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate)
出典と根拠
- ORDレコード
- ord-643f1dd86f91404aa5f5e314bc0f49bb
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07425634B2
関連ノート
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