Bromine → Methyl 5-bromo-2-hydroxy-4-methoxybenzoate

HRID 34962

反応式

HRID 34962 の反応式
[Br:1]Br.[CH3:3][O:4][C:5]1[CH:6]=[C:7]([OH:15])[C:8](=[CH:13][CH:14]=1)[C:9]([O:11][CH3:12])=[O:10]>C(Cl)Cl>[Br:1][C:14]1[CH:13]=[C:8]([C:9]([O:11][CH3:12])=[O:10])[C:7]([OH:15])=[CH:6][C:5]=1[O:4][CH3:3]

参加物

4

反応物 2

HCID 24408BromineHCID 79523Methyl 4-methoxysalicylate

生成物 1

HCID 1051517Methyl 5-bromo-2-hydroxy-4-methoxybenzoate収率 97%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 9.0 g (56.5 mmol) of bromine in 5 ml of CH2Cl2 is added dropwise to a 0° C. solution of 10.0 g (54.9 mmol) of methyl 4-methoxysalicylate in 90 ml of CH2Cl2. The reaction is stirred at 0° C. to 25° C. over five hours and then concentrated in vacuo to give 13.9 g of methyl 5-bromo-4-methoxysalicylate as a white solid: mp 141°-143° C.) (lit mp 143°-144° C.), Cresp, T. M.; Sargent, M. V.; Elix, J. A.; Murphy, D. P. H., J. Chem. Soc., Perkin Trans., 1, 1973, 340). The material is sufficiently pure to be used in the subsequent reaction.

後処理

  1. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c83c3657298944b6a8269e1c4ff4b7c4
出典データセット
uspto-grants-1988_08
特許番号
US04764525

関連ノート

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