3,5-Diaminobenzoic acid → 3,5-Bis(methoxyacetylamino)benzoic acid

HRID 1165881노트

반응식

HRID 1165881 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([NH2:11])[CH:10]=1)[C:5]([OH:7])=[O:6].[CH3:12][O:13][CH2:14][C:15](Cl)=[O:16]>N1C=CC=CC=1>[CH3:12][O:13][CH2:14][C:15]([NH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([NH:11][C:15](=[O:16])[CH2:14][O:13][CH3:12])[CH:10]=1)[C:5]([OH:7])=[O:6])=[O:16]

참가 물질

4

반응물 2

HCID 120623,5-Diaminobenzoic acidHCID 96623Methoxyacetyl chloride

생성물 1

HCID 146992893,5-Bis(methoxyacetylamino)benzoic acid

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of 3,5-diaminobenzoic acid (6.1 g) in pyridine (80 ml) is added dropwise methoxyacetyl chloride (8.0 ml) at room temperature, and the mixture is stirred for 2 hours as it stands. From the reaction mixture, pyridine is distilled off under reduced pressure. To the residue is added 1N hydrochloric acid, and the resulting solid substance is separated by filtration and washed with water. The resulting crude crystals are recrystallized from ethanol to give the title compound (8.0 g) having the following physical properties.

후처리

  1. distillationFrom the reaction mixture, pyridine is distilled off under reduced pressure
  2. additionTo the residue is added 1N hydrochloric acid
  3. customthe resulting solid substance is separated by filtration
  4. washwashed with water
  5. customThe resulting crude crystals are recrystallized from ethanol

출처 및 근거

ORD 기록
ord-c18d1b63afd146d5bc028e6dfcb1a481
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04912135

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