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Acetic Anhydride → N-(2-Chloro-4-iodophenyl)acetamide

HRID 1936395
ノート
印刷プレビュー

反応式

HRID 1936395 の反応式
[Cl:1][C:2]1[CH:8]=[C:7]([I:9])[CH:6]=[CH:5][C:3]=1[NH2:4].[C:10](OC(=O)C)(=[O:12])[CH3:11]>O1CCCC1>[Cl:1][C:2]1[CH:8]=[C:7]([I:9])[CH:6]=[CH:5][C:3]=1[NH:4][C:10](=[O:12])[CH3:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 2829302-Chloro-4-iodoaniline

生成物 1

HCID 18434368N-(2-Chloro-4-iodophenyl)acetamide収率 84%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

A solution of 2-chloro-4-iodoaniline (25 g, 96.66 mmol) in tetrahydrofuran (100 mL) was cooled to 0° C. and then treated with acetic anhydride (50.6 g, 500 mmol). The reaction mixture was stirred at 0° C. for 10 min and then allowed to warm to 25° C. where it was stirred for 15 h. The reaction mixture was then concentrated in vacuo to remove tetrahydrofuran. The residue was crystallized from ether (50 mL) and hexanes (50 mL). The solids were collected and washed with hexanes to afford N-(2-chloro-4-iodo-phenyl)-acetamide (23.87 g, 84%) as a white crystalline solid: EI-HRMS m/e calcd for C8H7ClINO (M+) 295.1526, found 295.1532.

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureto warm to 25° C. where it
  2. stirringwas stirred for 15 h
  3. concentrationThe reaction mixture was then concentrated in vacuo
  4. customto remove tetrahydrofuran
  5. customThe residue was crystallized from ether (50 mL) and hexanes (50 mL)
  6. customThe solids were collected
  7. washwashed with hexanes

出典と根拠

ORDレコード
ord-39989ddbf035457d89115e97c56a9806
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06388088B1

反応ノート

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