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

HRID 2427042노트

반응식

HRID 2427042 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 534416562-Amino-5-chloro-3-iodobenzoic acid수율 46.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-e5d6850f2ba34ce4bd3a6ea16293a89b
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07968573B2

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