Iodine chloride → 5-Chloro-2-iodo-4-(trifluoromethyl)aniline

HRID 2064128

반응식

HRID 2064128 반응식
[I:1]Cl.[Cl:3][C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][C:10]=1[C:11]([F:14])([F:13])[F:12])[NH2:7].O.O.O.C([O-])(=O)C.[Na+].C(=O)(O)[O-].[Na+].S([O-])([O-])=O.[Na+].[Na+]>C(O)(=O)C>[Cl:3][C:4]1[C:10]([C:11]([F:12])([F:13])[F:14])=[CH:9][C:8]([I:1])=[C:6]([CH:5]=1)[NH2:7]

참가 물질

6

반응물 4

HCID 24640Iodine chlorideHCID 679623-Chloro-4-(trifluoromethyl)anilineHCID 18470521HCID 18470521, 화합물HCID 23665404Sodium Acetate Trihydrate

생성물 1

HCID 593205585-Chloro-2-iodo-4-(trifluoromethyl)aniline

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Iodine monochloride (1.5 g) was added in one portion to a mixture of 3-chloro-4-trifluoromethylaniline (1.7 g), sodium acetate trihydrate (2.2 g), and acetic acid (10 ml) at room temperature. After 30 min aqueous sodium bicarbonate/sodium sulfite was added and the mixture extracted with diethyl ether. The organic phase was dried over Na2SO4, filtered and evaporated. The residue was purified by chromatography (ethyl acetate-hexane) to afford the title compound, 2.2 g.

후처리

  1. extractionthe mixture extracted with diethyl ether
  2. dry with materialThe organic phase was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. customThe residue was purified by chromatography (ethyl acetate-hexane)

출처 및 근거

ORD 기록
ord-b60f57e2e4c145499e75c59bc916ea89
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288412B2

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