反応式
C(P(CCCC)CCCC)CCC.[CH3:14][C:15]1[C:20]([CH2:21][OH:22])=[CH:19][CH:18]=[C:17]([C:23]([F:26])([F:25])[F:24])[N:16]=1.[CH3:27][O:28][C:29](=[O:43])[CH2:30][C:31]1[C:35]2[C:36]([CH3:42])=[CH:37][C:38](O)=[C:39]([CH3:40])[C:34]=2[S:33][CH:32]=1.C1CCN(C(N=NC(N2CCCCC2)=O)=O)CC1>C1COCC1>[CH3:27][O:28][C:29](=[O:43])[CH2:30][C:31]1[C:35]2[C:36]([CH3:42])=[CH:37][C:38]([O:22][CH2:21][C:20]3[C:15]([CH3:14])=[N:16][C:17]([C:23]([F:24])([F:26])[F:25])=[CH:18][CH:19]=3)=[C:39]([CH3:40])[C:34]=2[S:33][CH:32]=1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To a mixture of tri-n-butylphosphine (0.196 mL), (2-methyl-6-(trifluoromethyl)pyridin-3-yl)methanol (105 mg), methyl(6-hydroxy-4,7-dimethyl-1-benzothiophen-3-yl)acetate (130.9 mg) and THF (5.0 mL) was added ADDP (198 mg) at room temperature. The mixture was stirred at room temperature overnight under nitrogen atmosphere. The mixture was concentrated in vacuo. To the residue was added IPE, and the precipitate was filtered off. The filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (159 mg) as solid. The solid was crystallized from EtOAc-hexane.
後処理
- concentrationThe mixture was concentrated in vacuo
- additionTo the residue was added IPE
- filtrationthe precipitate was filtered off
- concentrationThe filtrate was concentrated in vacuo
- customThe residue was purified by silica gel column chromatography (EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-6ee8ad386e8b49789e726bac523dd442
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09238639B2
関連ノート
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