(4-Ethynylphenyl)(4-fluorophenyl)methanol → (4-Ethynylphenyl)(4-fluorophenyl)methanone
反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)[OH:10])=[CH:5][CH:4]=1)#[CH:2]>O1CCOCC1.O=[Mn]=O>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([C:9]([C:11]2[CH:12]=[CH:13][C:14]([F:17])=[CH:15][CH:16]=2)=[O:10])=[CH:7][CH:8]=1)#[CH:2]参加物
4
実験手順
The product of Step C was dissolved in anhydrous dioxane (20 ml) and to it MnO2 (0.5 g) was added. The suspension was stirred at reflux for 6 h and then filtered through Celite. The filtrate was distilled off and the residue was purified by FCC (SiO2) to give the product (0.18 g; 89%), as creamy paste. 1H-NMR (CDCl3) 3.24 (s, 1H); 7.15 (tr, 2H, J=8.73 Hz); 7.60 (d, 2H, J=6.69 Hz); 7.71 (d, 2H, J=6.58 Hz); 7.78-7.84 (m, 2H).
後処理
- additionwas added
- temperatureat reflux for 6 h
- filtrationfiltered through Celite
- distillationThe filtrate was distilled off
- customthe residue was purified by FCC (SiO2)
- customto give the product (0.18 g; 89%)
出典と根拠
- ORDレコード
- ord-a3f58eee58ab42aaa2844e2f227e4cea
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181182B2
反応ノート
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