HCID 16069467、化合物 → 5-Chloronaphthalene-2-carbonitrile
反応式
ClC(Cl)(Cl)C(O[C:6]1[CH:11]=C[C:9](C#N)=[CH:8][C:7]=1CC=C)=O.[Cl-:19].N1C=CC=CC=1CN1C=C[N+]([CH2:32][C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][N:34]=2)=C1>ClCCCl.Cl[Cu]>[Cl:19][C:6]1[CH:11]=[CH:32][CH:33]=[C:38]2[C:7]=1[CH:8]=[CH:9][C:36]([C:35]#[N:34])=[CH:37]2参加物
5
実験手順
A solution of INT 26 (1.01 g, 3.6 mmol) in degassed 1,2-dichloroethane (20 mL) containing CuCl (14.3 mg, 0.144 mmol) and 1,3-bis(pyridin-2-ylmethyl)-1H-imidazol-3-ium chloride (41.3 mg, 0.144 mmol, prepared according to: Journal of Organometallic Chemistry (2001), Vol. 617-618, 546-560.) was irradiated in the microwave for 2 hours at 200° C. and concentrated. The residue was purified by flash chromatography on silica gel (cyclohexane/EtOAc) to give INT 27.
後処理
- customwas irradiated in the microwave for 2 hours at 200° C.
- concentrationconcentrated
- customThe residue was purified by flash chromatography on silica gel (cyclohexane/EtOAc)
- customto give INT 27
出典と根拠
- ORDレコード
- ord-6958c70fe42f4eb1bce963ffec09a4b4
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08791100B2
反応ノート
読み込み中…