Hydrochloric Acid → HCID 11298899、化合物

HRID 458127ノート

反応式

HRID 458127 の反応式
[ClH:1].[C:2]([C:4]1[CH:13]=[CH:12][C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:6]([N+:14]([O-])=O)[CH:5]=1)#[N:3].[H][H]>CO.O=[Pt]=O>[Cl-:1].[NH2:14][C:6]1[CH:5]=[C:4]([CH:13]=[CH:12][C:7]=1[C:8]([O:10][CH3:11])=[O:9])[CH2:2][NH3+:3]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 11356202Methyl 4-cyano-2-nitrobenzoateHCID 178418361HCID 178418361、化合物3 回

生成物 1

HCID 11298899HCID 11298899、化合物

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 887Methanol溶媒

実験手順

After addition of 365 ml of concentrated hydrochloric acid (4.37 mol) and 9 g of PtO2, a suspension of 900 g (4.37 mol) of methyl 4-cyano-2-nitrobenzoate in 13.5 l of methanol is first hydrogenated at room temperature at a hydrogen pressure of 1 bar. After the hydrogen uptake has subsided, the pressure is increased to 17 bar, and hydorgenation is continued until the hydrogen uptake is complete. For work-up, the pressure is released to atmospheric pressure, the catalyst is removed by filtration through silica gel and the filtrate is concentrated completely in vacuo. Digestion of the residue with ethyl acetate yields 3-amino-4-methoxycarbonylbenzylammonium chloride, yield 757 g (80%), melting point 185–190° C. (decomp.).

後処理

  1. temperaturethe pressure is increased to 17 bar, and hydorgenation
  2. customthe catalyst is removed by filtration through silica gel
  3. concentrationthe filtrate is concentrated completely in vacuo

出典と根拠

ORDレコード
ord-17f0d40c44274d9ab707964f5f436a4a
出典データセット
uspto-grants-2007_03
特許番号
US07189848B2

反応ノート

読み込み中…