Hydrochloric Acid → HCID 11298899, 화합물

HRID 458127노트

반응식

HRID 458127 반응식
[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]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 11356202Methyl 4-cyano-2-nitrobenzoateHCID 178418361HCID 178418361, 화합물3회

생성물 1

HCID 11298899HCID 11298899, 화합물

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 887Methanol용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-17f0d40c44274d9ab707964f5f436a4a
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189848B2

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