反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]=[C:8]([CH:13]([CH3:17])[C:14]([OH:16])=O)[CH:7]=[CH:6]2.C(Cl)(=O)C(Cl)=O.[S:24]1[CH2:28][CH:27]([C:29]([OH:31])=[O:30])[NH:26][CH2:25]1.C(N(CC)CC)C.Cl>C1(C)C=CC=CC=1.CN(C)C=O.CC(C)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]=[C:8]([CH:13]([CH3:17])[C:14]([N:26]1[CH:27]([C:29]([OH:31])=[O:30])[CH2:28][S:24][CH2:25]1)=[O:16])[CH:7]=[CH:6]2参加物
反応物 5
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 0 °C
実験手順
To a solution of 6-methoxy-α-methyl-2-naphthalenacetic acid (4.02 g, 17.5 mmoles) in toluene (30 ml) and N,N-dimethylformamide (0.3 ml) cooled at 0° C., oxalylchloride (2.92 ml, 34.06 mmoles) is added. After 2 hours at room temperature, the solution is evaporated at reduced pressure. The obtained residue is dissolved in acetone (50 ml) and the solution is added to a solution of 4-thiazolidincarboxylic acid (2.33 g, 17.5 mmoles) and triethylamine (6.34 ml, 45.5 mmoles) in acetone (50 ml) cooled at 0° C. After 2 hours the solution is acidified with HCl 4 N, concentrated under vacuum, the residue is treated with ethyl acetate and the organic phase is washed first with HCl 2 N, then with water. The organic phase is anhydrified with sodium sulphate and evaporated at reduced pressure. 4.43 g of the expected product are obtained in the form of a white solid having m.p. 165° C.-168° C.
後処理
- customthe solution is evaporated at reduced pressure
- dissolutionThe obtained residue is dissolved in acetone (50 ml)
- concentrationconcentrated under vacuum
- additionthe residue is treated with ethyl acetate
- washthe organic phase is washed first with HCl 2 N
- customevaporated at reduced pressure
出典と根拠
- ORDレコード
- ord-5051bfc70c824566a78e478f7ef812aa
- 出典データセット
- uspto-grants-2008_07
- 特許番号
- US07402600B2
関連ノート
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