Benzoic acid, 4-amino-3-chloro-5-[(methoxyimino)methyl]-, methyl ester → 4-Amino-3-chloro-5-methoxyiminomethylbenzoic acid

HRID 583146

반응식

HRID 583146 반응식
[NH2:1][C:2]1[C:11]([CH:12]=[N:13][O:14][CH3:15])=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[CH:4][C:3]=1[Cl:16]>CO.[OH-].[Na+]>[NH2:1][C:2]1[C:11]([CH:12]=[N:13][O:14][CH3:15])=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[Cl:16]

참가 물질

4

반응물 1

HCID 53973576Benzoic acid, 4-amino-3-chloro-5-[(methoxyimino)methyl]-, methyl ester

생성물 1

HCID 540991344-Amino-3-chloro-5-methoxyiminomethylbenzoic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 14798Sodium Hydroxide용매

실험 절차

The methyl 4-amino-3-chloro-5-methoxyiminomethylbenzoate made in the previous step was dissolved in a mixture of 25 ml of methanol and 8 g ml of 10% of aqueous sodium hydroxide and the solution was then was refluxed for 2 hours. The methanol was removed using a rotary evaporator and the residue was partitioned between 25 ml of water and 25 ml of methylene chloride. To the cooled aqueous layer was added 6N aqueous hydrochloric acid, dropwise, with stirring, until the pH of mixture reached a value of 1. The resulting solid was filtered and dried yielding 1.4 g 4-amino-3-chloro-5-methoxyiminomethylbenzoic acid used without further purification.

후처리

  1. temperaturethe solution was then was refluxed for 2 hours
  2. customThe methanol was removed
  3. customa rotary evaporator
  4. customthe residue was partitioned between 25 ml of water and 25 ml of methylene chloride
  5. additionTo the cooled aqueous layer was added 6N aqueous hydrochloric acid
  6. filtrationThe resulting solid was filtered
  7. customdried

출처 및 근거

ORD 기록
ord-ce22cb967ea3459791869d17268ae29c
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05929098

연결된 노트

불러오는 중…