반응식
[F:1][C:2]1[CH:3]=[C:4]([C:10]2[CH:11]=[CH:12][C:13](=[O:16])[NH:14][N:15]=2)[CH:5]=[C:6]([F:9])[C:7]=1[F:8].O[CH2:18][C:19]1[CH:20]=[C:21]([C:25]2[N:30]=[CH:29][C:28](/[CH:31]=[CH:32]/[C:33]([O:35][CH3:36])=[O:34])=[CH:27][N:26]=2)[CH:22]=[CH:23][CH:24]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1>[O:16]=[C:13]1[N:14]([CH2:18][C:19]2[CH:20]=[C:21]([C:25]3[N:26]=[CH:27][C:28](/[CH:31]=[CH:32]/[C:33]([O:35][CH3:36])=[O:34])=[CH:29][N:30]=3)[CH:22]=[CH:23][CH:24]=2)[N:15]=[C:10]([C:4]2[CH:5]=[C:6]([F:9])[C:7]([F:8])=[C:2]([F:1])[CH:3]=2)[CH:11]=[CH:12]1참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
47.2 90 mg (0.4 mmol) of 6-(3,4,5-trifluorophenyl)-2H-pyridazin-3-one and 111 mg (0.41 mmol) of methyl (E)-3-[2-(3-hydroxymethylphenyl)pyrimidin-5-yl]acrylate are suspended in 3 ml of THF with 200 mg (0.6 mmol) of polymer-bound triphenylphosphine (about 3 mmol of triphenylphosphine per g), and the mixture is shaken at room temperature for 30 min. The mixture is cooled to 0° C., and 95 μl (0.6 mmol) of diethyl azodicarboxylate are added. The reaction mixture is shaken at room temperature for 24 h. The reaction mixture is purified by means of preparative HPLC; yield: 7 mg of “A283”; HPLC: Rt=3.41 min (method C); LC-MS: 479 (M+H).
후처리
- temperatureThe mixture is cooled to 0° C.
- stirringThe reaction mixture is shaken at room temperature for 24 h
- customThe reaction mixture is purified by means of preparative HPLC
출처 및 근거
- ORD 기록
- ord-24ba6300cd5b4f4b8023b62ee6449991
- 출처 데이터셋
- uspto-grants-2015_01
- 특허 번호
- US08927540B2
연결된 노트
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