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

HRID 724279

反応式

HRID 724279 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 218771372-(4-Methylsulfanyl-phenoxy)-nicotinic acid収率 94.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b6cd68847df546618176856ee718bfc1
出典データセット
uspto-grants-2006_11
特許番号
US07141586B2

関連ノート

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