反応式
[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH:2]1[C:11]([OH:13])=O.C[N:15]1[CH2:20][CH2:19][O:18]CC1.ClC(O[CH2:25][CH:26](C)[CH3:27])=O.C(N1[C:39]([NH2:40])=[C:38](N)[C:36](=[O:37])N(CCC)C1=O)CC.O1[CH2:49][CH2:48][CH2:47][CH2:46]1>C(OCC)C>[NH2:40][C:39]1[CH:38]([CH2:25][CH2:26][CH3:27])[C:36](=[O:37])[CH:46]([CH2:47][CH2:48][CH3:49])[C:19](=[O:18])[C:20]=1[NH:15][C:11]([CH:2]1[CH2:3][CH2:4][C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH2:1]1)=[O:13]参加物
反応物 5
生成物 1
試薬・触媒・溶媒 1
実験手順
Dissolve 1,2,3,4-tetrahydro-2-naphthoic acid (1.0 g, 5.67 mmol) in tetrahydrofuran (40 ml). Add N-methylmorpholine (0.62 ml, 5.67 mmol) and cool to -20° C. Add isobutyl chloroformate (0.73 ml, 5.67 mmol) and stir for 25 minutes. Then add 1,3-di-n-propyl-5,6-diaminouracil (1.28 g, 5.67 mmol, in 5 ml dimethylformamide) and stir the reaction for 5 hours at -20° C. Warm the reaction to room temperature and dilute with diethyl ether (300 ml). Separate the layers and rinse the organic layer with saturated sodium bicarbonate (200 ml), saturated sodium chloride solution (200 ml), dry over anhydrous magnesium sulfate, filter and concentrate. Purify the residue by radial chromatography (2% to 4% to 6% methanol/chloroform, 4 mm plate) to provide 1,2,3,4-tetrahydronaphthalene-2-carboxylic acid (2-amino-4,6-dioxo-3,5-dipropylcyclohex-1-enyl)amide (2.0 g) as a foam.
後処理
- customthe reaction for 5 hours at -20° C
- temperatureWarm
- customthe reaction to room temperature
- customSeparate the layers
- washrinse the organic layer with saturated sodium bicarbonate (200 ml), saturated sodium chloride solution (200 ml)
- dry with materialdry over anhydrous magnesium sulfate
- filtrationfilter
- concentrationconcentrate
- customPurify the residue by radial chromatography (2% to 4% to 6% methanol/chloroform, 4 mm plate)
出典と根拠
- ORDレコード
- ord-0d42d3e8acbb4e3db3bb6bef4ab7f44e
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05734052
関連ノート
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