Hydrochloric Acid → 3-(Methoxycarbonyl)-5-(N-methylmethylsulfonamido)benzoic acid

HRID 1160444ノート

反応式

HRID 1160444 の反応式
[CH3:1][N:2]([S:17]([CH3:20])(=[O:19])=[O:18])[C:3]1[CH:4]=[C:5]([C:13]([O:15][CH3:16])=[O:14])[CH:6]=[C:7]([CH:12]=1)[C:8]([O:10]C)=[O:9].[OH-].[K+].CO.Cl>O1CCCC1>[CH3:16][O:15][C:13]([C:5]1[CH:6]=[C:7]([CH:12]=[C:3]([N:2]([CH3:1])[S:17]([CH3:20])(=[O:19])=[O:18])[CH:4]=1)[C:8]([OH:10])=[O:9])=[O:14]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14797Potassium HydroxideHCID 11324067Dimethyl 5-(N-methylmethylsulfonamido)isophthalate

生成物 1

HCID 111503713-(Methoxycarbonyl)-5-(N-methylmethylsulfonamido)benzoic acid収率 95%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
90 °C

実験手順

A mixture of dimethyl 5-[methyl(methylsulfonyl)amino]isophthalate obtained in Reference Example 5 36.0 g (119 mmol), potassium hydroxide 8.71 g (155 mmol), methanol (360 mL) and tetrahydrofuran (240 mL) was stirred at 90° C. for 1.5 hours. To a mixture of 1N hydrochloric acid (200 mL) and ice water (500 mL) was added the reaction mixture dropwise, and the precipitated solid was collected by filtering, and dried under vacuum to give 32.4 g (113 mmol) of the title compound (yield: 95%).

後処理

  1. additionwas added the reaction mixture dropwise
  2. customthe precipitated solid was collected
  3. filtrationby filtering
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-559e6d83a0814b8bb9791a85a71cff52
出典データセット
uspto-grants-2010_10
特許番号
US07816387B2

反応ノート

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