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

Acetyl chloride → HCID 19349925、化合物

HRID 1672794
ノート
印刷プレビュー

反応式

HRID 1672794 の反応式
[OH:1][N:2]=[C:3]([NH2:11])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([I:10])[CH:5]=1.[C:12](Cl)(=O)[CH3:13]>N1C=CC=CC=1.C(OCC)(=O)C>[I:10][C:6]1[CH:5]=[C:4]([C:3]2[N:11]=[C:12]([CH3:13])[O:1][N:2]=2)[CH:9]=[CH:8][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6367Acetyl chlorideHCID 44235713-Iodo-N-hydroxy-benzamidine

生成物 1

HCID 19349925HCID 19349925、化合物収率 39%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

N′-Hydroxy-3-iodobenzamidine (1.80 g, 6.87 mmol) obtained in Step 1 was dissolved in pyridine (14 mL), and the mixture was stirred at room temperature for 1 hour after adding acetyl chloride (0.551 mL, 6.87 mmol). The mixture was cooled to room temperature after further stirring at 90° C. for 4 hours. After diluting the mixture with ethyl acetate, the organic layer was washed with 1 mol/L hydrochloric acid and saturated brine, and dried over anhydrous magnesium sulfate. The residue obtained upon concentration under reduced pressure was then purified by silica gel column chromatography to give 3-(3-iodophenyl)-5-methyl-1,2,4-oxadiazole (756 mg, 39%).

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. stirringafter further stirring at 90° C. for 4 hours
  3. washthe organic layer was washed with 1 mol/L hydrochloric acid and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe residue obtained upon concentration under reduced pressure
  6. customwas then purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-035e42d46afd4f1495ddc3813c4c0acd
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07998954B2

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