Potassium Carbonate → HCID 14373282, 화합물

HRID 414562

반응식

HRID 414562 반응식
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

참가 물질

7

반응물 3

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

생성물 1

HCID 14373282HCID 14373282, 화합물

시약·촉매·용매 3

HCID 6102075Dichlorobis(triphenylphosphine)palladium촉매HCID 1049Pyridine용매HCID 8471Triethylamine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-21b5abe2ce5d48d4b96e87aa7afe6b5e
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04792561

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