反応式
B1(B2C3CCCC2CCC3)C2CCCC1CCC2.C12CCCC(CCC1)B12[H]B2(C3CCCC2CCC3)[H]1.[CH3:39][O:40][C:41](=[O:45])[CH2:42][CH:43]=[CH2:44].ClCCl.[Br:49][C:50]1[CH:55]=[CH:54][CH:53]=[C:52](Br)[CH:51]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>O1CCCC1.[Pd](Cl)Cl.O.CN(C)C=O>[CH3:39][O:40][C:41](=[O:45])[CH2:42][CH2:43][CH2:44][C:52]1[CH:53]=[CH:54][CH:55]=[C:50]([Br:49])[CH:51]=1参加物
反応物 5
生成物 1
試薬・触媒・溶媒 4
実験手順
[9-Borabicyclo[3.3.1]nonane dimer] (13.4 mL, 6.68 mmol) (9-BBN dimer) was added to a solution of methyl-3-butenoate (0.71 mL, 6.68 mmol) in tetrahydrofuran (2.7 mL) at 0-5° C. under an argon atmosphere, and the mixture was stirred for 4 hours. N,N-Dimethylformamide (27 mL), palladium(II) chloride, dichloromethane (130 g, 0.16 mmol), 1,3-dibromobenzene (0.77 mL, 61.37 mmol) and potassium phosphate (powdered, 1.5 g, 6.94 mmol) were added. The mixture was treated at 50° C. overnight. Water was added and the mixture extracted with diethyl ether. The extract was washed with water, brine, and dried over sodium sulfate, and concentrated to dryness. Purification by flash chromatography, eluting with hexane/ethyl acetate) gave 4-(3-bromophenyl)butyric acid methyl ester as a clear oil (0.26 mg, 16%).
後処理
- additionThe mixture was treated at 50° C. overnight
- extractionthe mixture extracted with diethyl ether
- washThe extract was washed with water, brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated to dryness
- customPurification by flash chromatography
- washeluting with hexane/ethyl acetate)
出典と根拠
- ORDレコード
- ord-f2d14f1a6ab046f4bbd61fa0d584cbdd
- 出典データセット
- uspto-grants-2002_01
- 特許番号
- US06335459B1
関連ノート
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