Hydrochloric Acid → 2-Methyl-1,3-benzoxazole-4-carboxylic acid
反応式
[OH-].[K+].C([O:5][C:6]([C:8]1[CH:9]=[CH:10][CH:11]=[C:12]2[O:16][C:15]([CH3:17])=[N:14][C:13]=12)=[O:7])C.Cl>CO>[CH3:17][C:15]1[O:16][C:12]2[C:13](=[C:8]([C:6]([OH:7])=[O:5])[CH:9]=[CH:10][CH:11]=2)[N:14]=1参加物
5
実験手順
At 0° C. an aq. KOH solution (1.0M, 2.40 mL) is added to a solution of 2-methyl-benzooxazole-4-carboxylic acid ethyl ester (0.98 mmol) in MeOH (5.0 mL) and stirred for 30 min. The mixture is allowed to reach rt, stirred for additional 60 min and made acidic by addition of aq. hydrochloric acid (2.0 M). After removal of MeOH under reduced pressure the obtained precipitate is filtered off to give the desired product which is dried in vacuo. 1H-NMR (DMSO-d6): δ=2.64 (s, 3H); 7.41 (t, J=8.0 Hz, 1H); 7.83 (d, J=7.8 Hz, 1H); 7.88 (d, J=8.0 Hz, 1H); 12.8 (bs, 1H).
後処理
- customto reach rt
- stirringstirred for additional 60 min
- customAfter removal of MeOH under reduced pressure the obtained precipitate
- filtrationis filtered off
出典と根拠
- ORDレコード
- ord-bd690755fa9d4336a93624b3eb6a4a31
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08236801B2
反応ノート
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