Sodium Hydroxide → HCID 25140790、化合物
反応式
[OH-].[Na+].C[O:4][C:5]([C:7]1[C:8]2[CH:9]=[CH:10][CH2:11][O:12][C:13]=2[CH:14]=[CH:15][CH:16]=1)=[O:6]>CO.O>[O:12]1[C:13]2[CH:14]=[CH:15][CH:16]=[C:7]([C:5]([OH:6])=[O:4])[C:8]=2[CH:9]=[CH:10][CH2:11]1参加物
5
反応条件
- 温度
- 55 °C
実験手順
A solution of NaOH (7.26 mmol) in a mixture of MeOH (5.4 mL) and water (12.1 mL) is added to 2H-chromene-5-carboxylic acid methyl ester (4.84 mmol). The mixture is stirred at 55° C. for 3 h, partially concentrated in vacuo to remove MeOH and made acidic by addition of aq. HCl (1.0M). The desired carboxylic acid precipitates and is collected by filtration. 1H-NMR (DMSO-d6): δ=4.75 (bs, 2H); 5.99-6.05 (m, 1H); 6.98 (d, J=7.78 Hz, 1H); 7.19 (t, J=7.78 Hz, 1H); 7.25 (d, J=10.3 Hz, 1H); 7.40 (d, J=7.78 Hz, 1H); 13.0 (bs, 1H).
後処理
- concentrationpartially concentrated in vacuo
- customto remove MeOH
- additionmade acidic by addition of aq. HCl (1.0M)
- customThe desired carboxylic acid precipitates
- filtrationis collected by filtration
出典と根拠
- ORDレコード
- ord-51eb9de6abf2419891d6e598571b7524
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063099B2
反応ノート
読み込み中…