Water → 2,3-Diaminobenzoic acid

HRID 380516

반응식

HRID 380516 반응식
[N+:1]([C:4]1[C:12]([N+:13]([O-])=O)=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7])([O-])=O.Cl[Sn]Cl.O>C(O)(=O)C.Cl>[NH2:1][C:4]1[C:12]([NH2:13])=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7]

참가 물질

6

반응물 3

HCID 962WaterHCID 24479Stannous ChlorideHCID 2833272,3-Dinitrobenzoic acid

생성물 1

HCID 1980692,3-Diaminobenzoic acid수율 97.9%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매

실험 절차

To a suspension of 2 g (9.4 mmol) of 2,3-di-nitrobenzoic acid in 20 mL of acetic acid at 0° C. was added a solution of 14.8 g (65 mmol) SnCl2. 2 H2O in 7 mL of concentrated HCl. After stirring for 2 h at rt, the reaction mixture was concentrated. The residue was dissolved in 30 mL of H2O and the pH was adjusted to pH=12-13 with 6N NaOH. The mixture was filtered and the solid was washed with 0.1N HCl. The combined aqueous fractions were concentrated to give 1.4 g of the title compound.

후처리

  1. concentrationthe reaction mixture was concentrated
  2. dissolutionThe residue was dissolved in 30 mL of H2O
  3. filtrationThe mixture was filtered
  4. washthe solid was washed with 0.1N HCl
  5. concentrationThe combined aqueous fractions were concentrated

출처 및 근거

ORD 기록
ord-894b9a44de43464aad84271e1e113347
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06303593B1

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