Potassium Carbonate → HCID 14373282、化合物

HRID 414562

反応式

HRID 414562 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[O:12])[CH2:6][CH2:5]2.[CH2:13]([N:16]1[CH:20]=[CH:19][N:18]=[CH:17]1)[C:14]#[CH:15].C(=O)([O-])[O-].[K+].[K+]>N1C=CC=CC=1.C(N(CC)CC)C.[Pd](Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[N:16]1([CH2:13][C:14]#[C:15][C:2]2[CH:3]=[C:4]3[C:9](=[CH:10][CH:11]=2)[NH:8][C:7](=[O:12])[CH2:6][CH2:5]3)[CH:20]=[CH:19][N:18]=[CH:17]1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 125919421-(prop-2-yn-1-yl)-1H-imidazoleHCID 143732816-Bromo-3,4-dihydroquinolin-2(1H)-one

生成物 1

HCID 14373282HCID 14373282、化合物

試薬・触媒・溶媒 3

HCID 6102075Dichlorobis(triphenylphosphine)palladium触媒HCID 1049Pyridine溶媒HCID 8471Triethylamine溶媒

実験手順

A mixture of 11.6 mg of cuprous iodide, 86 mg of bis (triphenylphosphine) palladium (II) dichloride, 1.5 g of 6-bromo-3,4-dihydrocarbostyril and 774 mg of N-propargylimidazole was stirred in a mixture of 10 ml of pyridine and 2 ml of triethylamine at 100° C. for 48 hours under nitrogen. The reaction was then treated with 10 ml of saturated aqueous potassium carbonate and extracted with a solution of 10% methanol in methylene chloride. The extract was dried over anhydrous sodium sulfate, the solvent removed under reduced pressure and the residue chromatographed on silica gel eluting with 4% methanol in methylene chloride, yielding 6-[3-(imidazol-1-yl)-prop-1-yn-1-yl]-3,4-dihydrocarbostyril, m.p. 164°-168° C.

後処理

  1. extractionextracted with a solution of 10% methanol in methylene chloride
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. customthe solvent removed under reduced pressure
  4. customthe residue chromatographed on silica gel eluting with 4% methanol in methylene chloride

出典と根拠

ORDレコード
ord-21b5abe2ce5d48d4b96e87aa7afe6b5e
出典データセット
uspto-grants-1988_12
特許番号
US04792561

関連ノート

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