Lithium Hydroxide → 2-(4-Methylsulfanyl-phenoxy)-nicotinic acid

HRID 724279

반응식

HRID 724279 반응식
C[O:2][C:3](=[O:19])[C:4]1[CH:9]=[CH:8][CH:7]=[N:6][C:5]=1[O:10][C:11]1[CH:16]=[CH:15][C:14]([S:17][CH3:18])=[CH:13][CH:12]=1.[OH-].[Li+]>O1CCCC1>[CH3:18][S:17][C:14]1[CH:13]=[CH:12][C:11]([O:10][C:5]2[N:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([OH:19])=[O:2])=[CH:16][CH:15]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 587461792-(4-Methylsulfanyl-phenoxy)-nicotinic acid methyl ester

생성물 1

HCID 218771372-(4-Methylsulfanyl-phenoxy)-nicotinic acid수율 94.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2-(4-methylsulfanyl-phenoxy)-nicotinic acid methyl ester (10.36 g, 37.6 mmol) was dissolved in tetrahydrofuran (140 ml) and 1M aqueous lithium hydroxide solution (94 ml, 94 mmol) was added. The reaction was stirred at room temperature for 18 h and the tetrahydrofuran was removed under reduced pressure. The residue was acidified to pH1 with concentrated hydrochloric acid and the resulting precipitate was filtered, washed with water (2×10 ml), diethyether (3×10 ml) and dried in vacuo to give 2-(4-methylsulfanyl-phenoxy)-nicotinic acid (9.3 g) as a white solid.

후처리

  1. customthe tetrahydrofuran was removed under reduced pressure
  2. filtrationthe resulting precipitate was filtered
  3. washwashed with water (2×10 ml), diethyether (3×10 ml)
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-b6cd68847df546618176856ee718bfc1
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07141586B2

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