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1,4-Dioxane → HCID 57970213、化合物

HRID 1666633
ノート
印刷プレビュー

反応式

HRID 1666633 の反応式
Cl[C:2]1[CH:3]=[C:4]([CH3:11])[C:5]2[C:6](=[CH:8][S:9][CH:10]=2)[N:7]=1.Cl.[NH2:13][C@H:14]1[CH2:18][CH2:17][N:16]([C:19](=[O:32])[CH2:20][C:21]2[CH:26]=[CH:25][C:24]([O:27][C:28]([F:31])([F:30])[F:29])=[CH:23][CH:22]=2)[CH2:15]1.O1CCOCC1.CC(C)([O-])C.[Na+]>C(OCC)(=O)C.O.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]>[CH3:11][C:4]1[C:5]2[C:6](=[CH:8][S:9][CH:10]=2)[N:7]=[C:2]([NH:13][C@H:14]2[CH2:18][CH2:17][N:16]([C:19](=[O:32])[CH2:20][C:21]3[CH:22]=[CH:23][C:24]([O:27][C:28]([F:29])([F:30])[F:31])=[CH:25][CH:26]=3)[CH2:15]2)[CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 312751,4-DioxaneHCID 23676156Sodium t-butoxideHCID 552633012-Chloro-4-methylthieno[3,4-B]pyridineHCID 86636479(S)-1-(3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride

生成物 1

HCID 57970213HCID 57970213、化合物収率 26.8%

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

To a mixture of 2-chloro-4-methylthieno[3,4-b]pyridine (0.022 g), Pd2(dba)3 (0.005 g), (±)-BINAP (0.011 g), 1-((S)-3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride (0.046 g), and 1,4-dioxane (0.5 mL) was added sodium t-butoxide (0.045 g) under nitrogen atmosphere, and the mixture was stirred at 70° C. for 30 min. The reaction mixture was diluted with ethyl acetate and water, then the interlayer was removed by Celite filtration, and the organic layer was washed with saturated brine. The organic layer was dried with anhydrous magnesium sulfate, then the desiccant was removed by filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate/methanol=20:1, and silica gel, chloroform/methanol=20:1) to obtain light yellow oily (S)-1-(3-(4-methylthieno[3,4-b]pyridin-2-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (0.014 g).

後処理

  1. customthe interlayer was removed by Celite filtration
  2. washthe organic layer was washed with saturated brine
  3. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  4. customthe desiccant was removed by filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate/methanol=20:1, and silica gel, chloroform/methanol=20:1)

出典と根拠

ORDレコード
ord-f60673dc5a1f46ba859a7bdeef590394
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044068B2

反応ノート

読み込み中…

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