Dimethylformamide → 2-Amino-5-chloro-3-iodobenzoic acid

HRID 251932ノート

反応式

HRID 251932 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].CN(C)C=O.[I:17]N1C(=O)CCC1=O>O>[NH2:1][C:2]1[C:10]([I:17])=[CH:9][C:8]([Cl:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 124762-Amino-5-chlorobenzoic acidHCID 120273N-Iodosuccinimide

生成物 1

HCID 534416562-Amino-5-chloro-3-iodobenzoic acid収率 46.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of 1.5 g of 2-amino-5-chlorobenzoic acid and 100 ml of N,N-dimethylformamide was added 2.7 g of N-iodosuccinimide at room temperature, and the mixture was stirred at room temperature for 24 hours. After 30 ml of water was poured into the reaction mixture, the mixture was extracted with ethyl acetate three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 1.2 g of 2-amino-5-chloro-3-iodobenzoic acid of the formula:

後処理

  1. extractionthe mixture was extracted with ethyl acetate three times
  2. washwashed with an aqueous saturated sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-39fc76d62d1641d68479ea9a4f334cda
出典データセット
uspto-grants-2011_01
特許番号
US07867949B2

反応ノート

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