Hydrochloric Acid → Methyl 2-amino-4-{[(methylsulfonyl)amino]methyl}benzoate

HRID 458133ノート

反応式

HRID 458133 の反応式
[CH3:1][S:2]([NH:5][CH2:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([O:13][CH3:14])=[O:12])=[C:9]([N+:17]([O-])=O)[CH:8]=1)(=[O:4])=[O:3].Cl.[H][H]>CO.[Pd]>[NH2:17][C:9]1[CH:8]=[C:7]([CH2:6][NH:5][S:2]([CH3:1])(=[O:4])=[O:3])[CH:16]=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 22494948HCID 22494948、化合物HCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 11288376Methyl 2-amino-4-{[(methylsulfonyl)amino]methyl}benzoate収率 88%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

13.25 g (46 mmol) of methyl 4-methanesulfonylaminomethyl-2-nitrobenzoate are dissolved in 200 ml of methanol. After addition of 1.4 ml (46 mmol) of concentrated hydrochloric acid and 1 g of Pd catalyst (10% on active charcoal), the mixture is hydrogenated with hydrogen under atmospheric pressure until the hydrogen uptake is complete. The mixture is removed from the catalyst by filtration and the filtrate is concentrated completely. Crystallization of the residue from water yields 10.4 g (88%) of methyl 2-amino-4-methanesulfonylaminomethylbenzoate of melting point 121–122° C.

後処理

  1. customThe mixture is removed from the catalyst by filtration
  2. concentrationthe filtrate is concentrated completely
  3. customCrystallization of the residue from water

出典と根拠

ORDレコード
ord-d428dcd4e0cc49ccb3ef14c8f8eb218f
出典データセット
uspto-grants-2007_03
特許番号
US07189848B2

反応ノート

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