Sodium hydride → HCID 14277652, 화합물

HRID 35543

반응식

HRID 35543 반응식
Cl[C:2]1[C:7]([C:8]([OH:10])=[O:9])=[CH:6][N:5]=[CH:4][CH:3]=1.[CH3:11][O:12][C:13]1[CH:20]=[CH:19][C:16]([CH2:17][SH:18])=[CH:15][CH:14]=1.[H-].[Na+]>CN(C)C=O>[CH3:11][O:12][C:13]1[CH:20]=[CH:19][C:16]([CH2:17][S:18][C:2]2[C:7]([C:8]([OH:10])=[O:9])=[CH:6][N:5]=[CH:4][CH:3]=2)=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 804074-Methoxy-alpha-toluenethiolHCID 8182294-Chloronicotinic acid

생성물 1

HCID 14277652HCID 14277652, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A stirred and ice-cooled mixture of 788 mg (0.005 mole) 4-chloronicotinic acid [prepared by the process set forth in W. C. J. Ross, J. Chem. Soc.(C), 1816 (1966)]and 771 mg (0.005 mole) of 4-methoxybenzylmercaptan in 6 mL of dry N,N-dimethylformamide was treated with 480 mg (0.012 mole) of 60% sodium hydride dispersion. The reaction was stirred at room temperature for 4 hours during which a thick solid formed, which was taken up in 75 mL of ice water. After extraction with 25 mL of hexane, the aqueous layer was acidified with 2.5N hydrochloric acid to precipitate 4-(4-methoxybenzylthio)-nicotinic acid; yield 1.2 g (89% of theory), m.p. 230° C.

후처리

  1. temperatureice-cooled
  2. customprepared by the process
  3. stirringThe reaction was stirred at room temperature for 4 hours during which a thick solid
  4. customformed
  5. extractionAfter extraction with 25 mL of hexane
  6. customto precipitate 4-(4-methoxybenzylthio)-nicotinic acid

출처 및 근거

ORD 기록
ord-38fb0fdd2a2f47e8aaff7fe85e841c20
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04767766

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