2-(4-Bromobenzyl)malonic acid → 3-(4-Bromophenyl)propionic acid
反応式
[Br:1][C:2]1[CH:15]=[CH:14][C:5]([CH2:6][CH:7](C(O)=O)[C:8]([OH:10])=[O:9])=[CH:4][CH:3]=1>CS(C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][CH2:7][C:8]([OH:10])=[O:9])=[CH:14][CH:15]=1参加物
3
実験手順
A solution of 2-(4-bromobenzyl)malonic acid (18 g, 66.18 mmol, 1.00 equiv) in dimethylsulfoxide (50 mL) was stirred at 160° C. for 2 h. The reaction mixture was cooled to room temperature and the product was precipitated by the addition of 200 mL ice and water. The solid was collected by filtration, washed with 1×50 mL of water and dried in a vacuum oven to give 14.8 g (98%) of 3-(4-bromophenyl)propanoic acid as a white solid. LC-MS: (ES, m/z): 229 [M+H]+. 1HNMR (400 MHz, DMSO-d6, ppm): δ 7.45 (d, J=8.0 Hz, 2H), 7.21 (d, J=8.0 Hz, 2H), 2.82-2.77 (m, 2H), 2.55-2.51 (m, 2H).
後処理
- customthe product was precipitated by the addition of 200 mL ice and water
- filtrationThe solid was collected by filtration
- washwashed with 1×50 mL of water
- customdried in a vacuum oven
出典と根拠
- ORDレコード
- ord-45abe453f59540788b1afb94807d32ff
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09296732B2
反応ノート
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