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HCID 67260634、化合物 → HCID 178510668、化合物

HRID 2359052
ノート
印刷プレビュー

反応式

HRID 2359052 の反応式
Br[C:2]1[N:6](CC2C=CC(OC)=CC=2)[N:5]=[C:4]([C:16]2[S:17][C:18]([Cl:21])=[CH:19][CH:20]=2)[C:3]=1[C:22]1[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=1.Br[C:29]1C(C2C=CN=CC=2)=C(C2SC(Cl)=CC=2)N(CC2C=CC(OC)=CC=2)[N:30]=1>CN(C)C=O.O.C(OCC)(=O)C.[C-]#N.[Zn+2].[C-]#N.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:21][C:18]1[S:17][C:16]([C:4]2[C:3]([C:22]3[CH:23]=[CH:24][N:25]=[CH:26][CH:27]=3)=[C:2]([C:29]#[N:30])[NH:6][N:5]=2)=[CH:20][CH:19]=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 2

HCID 67260634HCID 67260634、化合物HCID 67261945HCID 67261945、化合物

生成物 1

HCID 178510668HCID 178510668、化合物収率 15%

試薬・触媒・溶媒 5

HCID 11186Zinc cyanide (Zn(CN)2)触媒HCID 178418397HCID 178418397、化合物触媒
HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
160 °C

実験手順

To 4-[5-bromo-3-(5-chloro-2-thienyl)-1-(4-methoxybenzyl)-1H-pyrazol-4-yl]pyridine and 4-[3-bromo-5-(5-chloro-2-thienyl)-1-(4-methoxybenzyl)-1H-pyrazol-4-yl]pyridine (mixture of isomers 2:1, 1 eq, 0.435 mmol) in 1 mL of N,N-dimethylformamide, were added zinc cyanide (0.65 mmol) and Tetrakis(triphenylphosphine)palladium(0) (0.09 mmol). The mixture was stirred for 5 mins at 160° C. in the microwave. After cooling to room temperature, the reaction mixture was diluted with water and ethyl acetate was added. The aqueous layer was extracted with ethyl acetate and the combined organic extracts were dried over MgSO4, filtered and concentrated. The residue was dissolved in 1 mL of trifluoroacetic acid and stirred at 65° C. for 2 h. Water and ethyl acetate were added. And the aqueous layer was extracted with ethyl acetate. The combined organic extracts were washed with a saturated solution of sodium hydrogen carbonate, dried over MgSO4, filtered and concentrated. The residue was purified by chromatography on silica gel (dichloromethane/methanol 20:1 to 10:1) to afford 19 mg of 3-(5-chloro-2-thienyl)-4-(pyridin-4-yl)-1H-pyrazole-5-carbonitrile (15% yield).

後処理

  1. temperatureAfter cooling to room temperature
  2. additionwas added
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. dry with materialthe combined organic extracts were dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. dissolutionThe residue was dissolved in 1 mL of trifluoroacetic acid
  8. stirringstirred at 65° C. for 2 h
  9. additionWater and ethyl acetate were added
  10. extractionAnd the aqueous layer was extracted with ethyl acetate
  11. washThe combined organic extracts were washed with a saturated solution of sodium hydrogen carbonate
  12. dry with materialdried over MgSO4
  13. filtrationfiltered
  14. concentrationconcentrated
  15. customThe residue was purified by chromatography on silica gel (dichloromethane/methanol 20:1 to 10:1)

出典と根拠

ORDレコード
ord-9bfa95ee76a742ffbf4fb36da4001a09
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08685974B2

反応ノート

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