Diisopropylethylamine → HCID 66765112、化合物
反応式
[CH2:1]([O:3][C:4](=[O:14])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7](Br)[CH:6]=1)[CH3:2].[CH2:15]([O:23][C:24](=[O:28])[CH2:25][CH2:26][SH:27])[CH2:16][CH2:17][CH2:18][CH2:19][CH:20]([CH3:22])C.[CH:29](N(C(C)C)CC)(C)C.CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH2:1]([O:3][C:4](=[O:14])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([S:27][CH2:26][CH2:25][C:24]([O:23][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:22][CH3:29])=[O:28])[CH:6]=1)[CH3:2]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 90 °C
実験手順
3-Bromo-4-methoxy-benzoic acid ethyl ester (1.61 g, 6.62 mmol) and isooctyl-3-mercaptopropionate (1.73 g, 7.95 mmol) were dissolved in dioxane (26 mL) and the mixture was sparged with N2 (g) for 10 minutes. Diisopropylethyl amine (2.31 mL, 13.25 mmol), Xanthphos (0.1917 g, 0.33 mmol) and tris(dibenzylideneacetone)dipalladium(0) (0.1517 g, 0.166 mmol) were added and the mixture was sparged with N2 (g) for 5 minutes. The reaction was then heated to 90° C. for 2 hours after which time it was filtered to remove solid impurities. The mixture was concentrated and the residue was purified on silica gel (0-40% EtOAc in hexanes) to give the title compound.
後処理
- customthe mixture was sparged with N2 (g) for 10 minutes
- customthe mixture was sparged with N2 (g) for 5 minutes
- filtrationwas filtered
- customto remove solid impurities
- concentrationThe mixture was concentrated
- customthe residue was purified on silica gel (0-40% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-ec88ccc5db564be69341524009f9268d
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US09000025B2
反応ノート
読み込み中…