Hydrochloric Acid → Acetic acid, 2-((2-chlorobenzoyl)amino)-

HRID 44438ノート

反応式

HRID 44438 の反応式
[NH2:1][CH2:2][C:3]([OH:5])=[O:4].[OH-].[Na+].[Cl:8][C:9]1[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=1[C:11](Cl)=[O:12].Cl>O>[Cl:8][C:9]1[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=1[C:11]([NH:1][CH2:2][C:3]([OH:5])=[O:4])=[O:12]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 750GlycineHCID 14798Sodium HydroxideHCID 691102-Chlorobenzoyl chloride

生成物 1

HCID 177756Acetic acid, 2-((2-chlorobenzoyl)amino)-収率 80%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred solution of glycine (100 mmol) and NaOH (100 mmol) in water (300 ml), at 5° C., o-chloro-benzoyl chloride (110 mmol) was added in small portions. The reaction mixture was stirred for 30 minutes at room temperature, then cooled again and acidified to pH=2 by addition of 6 M HCl. Extraction of the aqueous solution was performed with EtOAc. Then, the combined organic layers were dried over MgSO4 and the solvent was removed by reduced pressure. The residue was triturated in boiling chloroform, and the product was collected by filtration in 80% yield.

後処理

  1. temperaturecooled again
  2. extractionExtraction of the aqueous solution
  3. dry with materialThen, the combined organic layers were dried over MgSO4
  4. customthe solvent was removed by reduced pressure
  5. customThe residue was triturated
  6. filtrationthe product was collected by filtration in 80% yield

出典と根拠

ORDレコード
ord-4a9fdad254f04dc1b4dd32db485b3fe6
出典データセット
uspto-grants-2013_09
特許番号
US08541428B2

反応ノート

読み込み中…