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Chlorotrimethylsilane → (4-(1H-indol-5-yloxy)pyrimidin-2-yl)methyl acetate

HRID 45173
ノート
印刷プレビュー

反応式

HRID 45173 の反応式
BrCCBr.Cl[Si](C)(C)C.[C:10]([O:13][CH2:14]Br)(=[O:12])[CH3:11].Cl[C:17]1[N:22]=[C:21]([O:23][C:24]2[CH:25]=[C:26]3[C:30](=[CH:31][CH:32]=2)[NH:29][CH:28]=[CH:27]3)[CH:20]=[CH:19][N:18]=1>CN(C=O)C.C(Cl)Cl.[Zn].C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[C:10]([O:13][CH2:14][C:17]1[N:22]=[C:21]([O:23][C:24]2[CH:25]=[C:26]3[C:30](=[CH:31][CH:32]=2)[NH:29][CH:28]=[CH:27]3)[CH:20]=[CH:19][N:18]=1)(=[O:12])[CH3:11]
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

9

反応物 4

HCID 6397ChlorotrimethylsilaneHCID 78391,2-DibromoethaneHCID 68536Bromomethyl acetateHCID 577373465-(2-chloropyrimidin-4-yloxy)-1H-indole2 回

生成物 1

HCID 59394351(4-(1H-indol-5-yloxy)pyrimidin-2-yl)methyl acetate

試薬・触媒・溶媒 4

HCID 23994Zinc触媒
HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒
HCID 6228Dimethylformamide溶媒2 回
HCID 6344Dichloromethane溶媒2 回

反応条件

温度
60 °C

実験手順

To a suspension of nano zinc metallic powder (Strem Chemicals; average particle size 75-125 nm) (1.34 g, 20.52 mmol) in DMF (8 ml) is added 1,2-dibromoethane (0.19 mL, 2.2 mmol). The heterogeneous mixture is heated to 60° C. and then stirred for 10 min. The mixture is cooled to room temperature and charged with chlorotrimethylsilane (0.24 mL, 1.8 mmol). The reaction vessel is then sonicated in a room temperature water bath for 30 min. The suspension is then left standing for ca. 30 min to permit the solid to settle and the supernatant is then removed via syringe. DMF (8 ml) is then added, followed by bromomethyl acetate (1.00 mL, 10.3 mmol). The reaction mixture is then stirred for 2 hr at room temperature. The suspension is then left standing for 1 hour to permit the solid to settle. Next a separate flask is charged with 5-(2-chloropyrimidin-4-yloxy)-1H-indole (450 mg, 1.83 mmol), prepared as described in Example 73-A, DMF (3 mL) is then added to the 5-(2-chloropyrimidin-4-yloxy)-1H-indole followed by Pd(dppf)Cl2.CH2Cl2 (230 mg, 0.28 mmol). To this solution is added a portion of the supernatant (6 mL), from the flask containing the organozincate, via syringe. The reaction is heated at 50° C. for 16 h then cooled to room temperature and diluted with DCM and saturated aqueous NH1Cl. The layers are separated and the aqueous layer is extracted 2 additional times with DCM. The organic layers are combined dried over anhydrous Na2SO4, filtered, and concentrated.

後処理

  1. temperatureThe mixture is cooled to room temperature
  2. customThe reaction vessel is then sonicated in a room temperature water bath for 30 min
  3. waitThe suspension is then left
  4. waitstanding for ca. 30 min
  5. customthe supernatant is then removed via syringe
  6. additionDMF (8 ml) is then added
  7. stirringThe reaction mixture is then stirred for 2 hr at room temperature
  8. waitThe suspension is then left
  9. waitstanding for 1 hour
  10. customprepared
  11. additionTo this solution is added a portion of the supernatant (6 mL)
  12. additionfrom the flask containing the organozincate
  13. temperatureThe reaction is heated at 50° C. for 16 h
  14. temperaturethen cooled to room temperature
  15. customThe layers are separated
  16. extractionthe aqueous layer is extracted 2 additional times with DCM
  17. dry with materialThe organic layers are combined dried over anhydrous Na2SO4
  18. filtrationfiltered
  19. concentrationconcentrated

出典と根拠

ORDレコード
ord-8123e138a20e4c2bb38d0ed82b487dbd
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08541432B2

反応ノート

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