Hydrochloric Acid → 6-Amino-2-methyl-3-nitrobenzoic acid

HRID 22181

반응식

HRID 22181 반응식
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([NH:14]C(=O)C)=[C:8]([C:12]=1[CH3:13])[C:9]([OH:11])=[O:10])([O-:3])=[O:2].Cl>[OH-].[Na+]>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([NH2:14])=[C:8]([C:12]=1[CH3:13])[C:9]([OH:11])=[O:10])([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 152831716-Acetylamino-2-methyl-3-nitro-benzoic acid

생성물 1

HCID 152831726-Amino-2-methyl-3-nitrobenzoic acid수율 48%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

A solution of 10.2 g (43 mmoles) of 5-nitro-6-methyl-2-acetylaminobenzoic acid in 100 mL of 2M NaOH was heated to reflux for two hours. The resultant red solution was allowed to cool to near room temperature, then transferred to a beaker sitting in an ice bath. The solution was slowly acidified with 2N HCl to a pH of approximately 4-5 when a voluminous yellow solid separated out. In all, approximately 110 mL of 2N HCl was added. The collected yellow solid was dried in a vacuum oven for 3 hours at 75 degrees. 4.0 g (48% yield) 5-nitro-6-methyl-2-aminobenzoic acid was obtained. NMR(DMSO-d6): 2.45 (s,3H), 3.35(bs,2H), 6.68(d,1H,J=9.0 Hz), 7.86(d,1H,J=9.0 Hz). MS(m/z): 196(M+).

후처리

  1. temperatureto reflux for two hours
  2. customsitting in an ice bath
  3. customseparated out
  4. additionIn all, approximately 110 mL of 2N HCl was added
  5. customThe collected yellow solid was dried in a vacuum oven for 3 hours at 75 degrees

출처 및 근거

ORD 기록
ord-adeba882874f41c2af6f5027a5fb944a
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05428021

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