Methyl 4-amino-3-chloro-5-methoxyiminomethylbenzoate → 4-Amino-3-chloro-5-methoxyiminomethylbenzoic acid

HRID 583146ノート

反応式

HRID 583146 の反応式
[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]

参加物

4

反応物 1

HCID 53973576Methyl 4-amino-3-chloro-5-methoxyiminomethylbenzoate

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ce22cb967ea3459791869d17268ae29c
出典データセット
uspto-grants-1999_07
特許番号
US05929098

反応ノート

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