Water → HCID 12901252、化合物

HRID 1589207ノート

反応式

HRID 1589207 の反応式
[NH2:1][C:2]1[C:7]([C:8](=[O:16])[C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:17][C:18]([OH:20])=[O:19].[Na].O.[CH2:23](I)[CH3:24]>CN(C)C=O>[NH2:1][C:2]1[C:7]([C:8](=[O:16])[C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:17][C:18]([O:20][CH2:23][CH3:24])=[O:19]

参加物

6

反応物 4

HCID 962Water2 回HCID 6340IodoethaneHCID 173842Ahr 6293HCID 5360545Sodium

生成物 1

HCID 12901252HCID 12901252、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Fourteen g of 2-amino-3-(4-chlorobenzoyl)benzene acetic acid, sodium salt.H2O was dissolved in 150 ml of dimethylformamide and then treated with 30 g of ethyl iodide. The resulting solution was stirred at room temperature for 2.5 hours. The solution was then added to water and the mixture was extracted several times with benzene. The benzene layer obtained was washed with dilute base and water, dried over sodium sulfate and stripped to leave an oil which crystallized on trituration with pet. ether. Recrystallization from ethyl alcohol gave 11.6 g of the titled compound as yellow flakes, m.p. 101°-102° C.

後処理

  1. extractionthe mixture was extracted several times with benzene
  2. customThe benzene layer obtained
  3. washwas washed
  4. additionwith dilute base and water
  5. dry with materialdried over sodium sulfate
  6. customto leave an oil which
  7. customcrystallized on trituration with pet. ether
  8. customRecrystallization from ethyl alcohol

出典と根拠

ORDレコード
ord-87062308bf374ce2830aa886862b8b8b
出典データセット
uspto-grants-1986_02
特許番号
US04568695

反応ノート

読み込み中…