反応式
[CH3:1][S:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=O)=[CH:5][CH:4]=1.Cl.CN(C)CCN=C=NCC.[NH:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1>C1COCC1>[CH3:1][S:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)=[O:9])=[CH:10][CH:11]=1参加物
5
実験手順
To a stirred solution of 4-(methylthio)benzoic acid (6.76 g, 40.2 mmol) and N-[2-(dimethylamino)ethyl]-N′-ethylcarbodiimide hydrochloride (9.24 g, 48.2 mmol) in THF (100 mL) was added morpholine (4.2 mL, 48.2 mmol). After stirring for 2 hours, the reaction was concentrated in vacuo and the residue partitioned between ethyl acetate (100 mL) and 2M hydrochloric acid (150 mL). The organic phase was separated, washed with 1M aqueous sodium carbonate solution, dried over sodium sulfate, filtered and concentrated in vacuo to give the title compound LC retention time 3.52 mins MS m/z 238 (MH+).
後処理
- concentrationthe reaction was concentrated in vacuo
- customthe residue partitioned between ethyl acetate (100 mL) and 2M hydrochloric acid (150 mL)
- customThe organic phase was separated
- washwashed with 1M aqueous sodium carbonate solution
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-037be1b1b0ef41ba93b21ed6ef1338dd
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07446117B2
関連ノート
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