Water → 3-Iodo-4-methylbenzoic acid
反応式
C[O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[C:6]([I:11])[CH:5]=1.[OH-].[Na+].O>CO>[I:11][C:6]1[CH:5]=[C:4]([CH:9]=[CH:8][C:7]=1[CH3:10])[C:3]([OH:12])=[O:2]参加物
5
実験手順
Methyl-3-Iodo-4-methylbenzoate (3 g, 109 mmol, 1 eq) dissolved in MeOH (30 ml) was added sodium hydroxide (1.3 g, 327 mmol, 3 eq) followed by the addition of water (15 ml). The above solution was stirred at room temperature for 14 h. The solution was concentrated under vacuum, and then added water. The pH of the reaction was bought to 3 using Conc.HCl. The solid obtained was filtered and dried under vacuum. Yield: 2.7 g (96%). 1HNMR (400 MHz, DMSO-d6): δ 2.44 (s, 3H), 7.45 (d, J=8.00 Hz, 1H), 7.85 (d, J=3.18 Hz, 1H), 8.31 (s, 1H).
後処理
- concentrationThe solution was concentrated under vacuum
- customThe solid obtained
- filtrationwas filtered
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-4e88ff1604a94ca7b5dd632420ca3b1e
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08536338B2
反応ノート
読み込み中…