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Hydrochloric Acid → 7-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-3-(2-methylphenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine

HRID 1893423
ノート
印刷プレビュー

反応式

HRID 1893423 の反応式
[Cl:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[C:12]([N:14]1[CH2:19][CH2:18][N:17]2[CH:20]=[CH:21][N:22]=[C:16]2[CH2:15]1)=[O:13].Br[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[CH3:30].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+].Cl>O1CCOCC1.ClCCl.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(OCC)C>[Cl:1][C:2]1[C:7]([C:8]([F:9])([F:10])[F:11])=[CH:6][CH:5]=[CH:4][C:3]=1[C:12]([N:14]1[CH2:19][CH2:18][N:17]2[C:20]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[CH3:30])=[CH:21][N:22]=[C:16]2[CH2:15]1)=[O:13]
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

10

反応物 5

HCID 313Hydrochloric AcidHCID 72362-BromotolueneHCID 10796Cesium carbonateHCID 11776TriphenylphosphineHCID 497850107-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine

生成物 1

HCID 49785368
7-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-3-(2-methylphenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine
収率 5.92%

試薬・触媒・溶媒 4

HCID 167845palladium(II) acetate触媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
90 °C

実験手順

7-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine (0.330 g, 1 mmol, Example 1), 1-bromo-2-methylbenzene (0.132 mL, 1.100 mmol), palladium(II)acetate (0.011 g, 0.050 mmol), triphenylphosphine (0.026 g, 0.100 mmol) and cesium carbonate (0.342 g, 1.050 mmol) were suspended in 1,4-dioxane (5 ml) under argon. The mixture was degassed 3 times and heated at 90° C. for 16 h. The solvent was removed in vacuo and the residue partitioned between ethyl acetate (50 ml) and water (50 ml). The aqueous phase was extracted with ethyl acetate (2×50 ml), the combined organic extracts were washed with water (3×50 ml), brine (50 ml) dried over anhydrous sodium sulfate and concentrated to a crude oil. The crude oil was purified by mass-directed automated preparative HPLC to afford the free base that was dissolved in dichloromethane (5 ml) and treated with 4N HCl in dioxane. The solvents were removed in vacuo and the solid tritruated with diethyl ether to afford 7-{[2-chloro-3-(trifluoromethyl)phenyl]carbonyl}-3-(2-methylphenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine (0.027 g, 0.059 mmol, 5.92% yield).

後処理

  1. customThe mixture was degassed 3 times
  2. customThe solvent was removed in vacuo
  3. customthe residue partitioned between ethyl acetate (50 ml) and water (50 ml)
  4. extractionThe aqueous phase was extracted with ethyl acetate (2×50 ml)
  5. washthe combined organic extracts were washed with water (3×50 ml), brine (50 ml)
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated to a crude oil
  8. customThe crude oil was purified
  9. customto afford the free base that
  10. customThe solvents were removed in vacuo

出典と根拠

ORDレコード
ord-ea37b71eb32d4cd293262fa46067e466
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08513248B2

反応ノート

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