ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium Iodide → HCID 19905868、化合物

HRID 904942
ノート
印刷プレビュー

反応式

HRID 904942 の反応式
[CH3:1][CH2:2][NH:3][CH2:4][CH2:5][NH:6][C:7]([C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]([CH3:18])=[O:17])=[CH:11][CH:10]=1)=[O:8].Cl[CH2:20][C:21](Cl)=O.[I-].[Na+].[OH-:26].[NH4+:27]>CC(C)=O.CO>[C:16]([NH:15][C:12]1[CH:11]=[CH:10][C:9]([C:7]([NH:6][CH2:5][CH2:4][N:3]([CH2:20][CH3:21])[C:2](=[O:26])[CH2:1][NH2:27])=[O:8])=[CH:14][CH:13]=1)(=[O:17])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 6577Chloroacetyl chlorideHCID 14923Ammonium HydroxideHCID 155689Desethyl-N-acetylprocainamide

生成物 1

HCID 19905868HCID 19905868、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒2 回
HCID 887
Methanol
溶媒
2 回

実験手順

A mixture containing desethyl-N-acetyl procainamide (1.25 g) (prepared as in Example VII and 0.8 g of chloroacetyl chloride dissolved in 25 ml of acetone was refluxed for two hours. The reaction mixture was filtered and the filtrate evaporated to yield a yellow residue. The yellow residue and 0.75 g of sodium iodide were dissolved in 20 ml of acetone and refluxed for one hour. The resulting mixture was filtered and the filtrate evaporated to dryness to yield a red residue which was then dissolved in 20 ml of methanol. To the methanol solution was added 20 ml of concentrated ammonium hydroxide and the resulting mixture was refluxed for 1.5 hours. The mixture was cooled and then extracted twice with 20 ml of chloroform. The combined extracts were dried over sodium sulfate, filtered and evaporated to yield N-p-acetamidobenzoyl-N'-ethyl-N'-aminoacetylethylene diamine. To 10 mg of N-p-acetamidobenzoyl-N'-ethyl-N'-aminoacetylethylene diamine was added 10 mg of 5-[(4,6-dichlorotriazin-2-yl)-amino]fluorescein dissolved in 1 ml of methanol and the reaction was allowed to proceed for ten minutes until a crude product had formed. The crude product was purified using silica gel thin-layer chromatographic techniques employing a developing solvent comprising a 1:1 mixture of chloroform:acetone to yield an N-P-acetamidobenzoyl-N'-ethyl-N'-aminoacetylethylene diamine-DTAF conjugate of the formula: ##STR10##

後処理

  1. temperaturewas refluxed for two hours
  2. filtrationThe reaction mixture was filtered
  3. customthe filtrate evaporated
  4. customto yield a yellow residue
  5. temperaturerefluxed for one hour
  6. filtrationThe resulting mixture was filtered
  7. customthe filtrate evaporated to dryness
  8. customto yield a red residue which
  9. temperaturethe resulting mixture was refluxed for 1.5 hours
  10. temperatureThe mixture was cooled
  11. extractionextracted twice with 20 ml of chloroform
  12. dry with materialThe combined extracts were dried over sodium sulfate
  13. filtrationfiltered
  14. customevaporated

出典と根拠

ORDレコード
ord-80c17ffc8ce3446ea137cd3740cb075c
出典データセット
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04420568

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート