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Iodine → Methyl 2-amino-4-chloro-5-iodobenzoate

HRID 1857629
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반응식

HRID 1857629 반응식
[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[CH:6][C:5]=1[NH:11]C(=O)C.[I:16]I>FC(F)(F)C([O-])=O.[Ag+]>[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([I:16])[C:7]([Cl:10])=[CH:6][C:5]=1[NH2:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 807IodineHCID 2800203Benzoic acid, 2-(acetylamino)-4-chloro-, methyl ester

생성물 1

HCID 10852539Methyl 2-amino-4-chloro-5-iodobenzoate수율 82.6%

시약·촉매·용매 1

HCID 76299Silver trifluoroacetate촉매

실험 절차

To a suspension of 2-acetylamino-4-chlorobenzoic acid methyl ester (2.0 g in 80 mL of dry chloroform) and 2.5 g silver trifluoroacetate was added iodine (2.87 g in 40 mL chloroform) and the mixture stirred at room temperature. After 5 hours, the mixture was filtered over diatomaceous earth and the filtrate concentrated in vacuo. Purification of the resulting oil by flash chromatography on silica gel (hexane:ethyl acetate, 95:5; then 90:10) gave the title compound (2.26 g).

후처리

  1. filtrationthe mixture was filtered over diatomaceous earth
  2. concentrationthe filtrate concentrated in vacuo
  3. customPurification of the resulting oil by flash chromatography on silica gel (hexane

출처 및 근거

ORD 기록
ord-034b90ab6aed494aa691454dfa215d2f
출처 데이터셋
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06147088

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