4-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotoluene → 1-Hydroxy-6-(trifluoromethyl)benzotriazole

HRID 10755

반응식

HRID 10755 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=O.O.[NH2:16][NH2:17]>C(O)C>[OH:14][N:12]1[C:3]2[CH:4]=[C:5]([C:8]([F:11])([F:10])[F:9])[CH:6]=[CH:7][C:2]=2[N:17]=[N:16]1

참가 물질

4

반응물 2

HCID 84624-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotolueneHCID 24654Hydrazine hydrate (1:1)

생성물 1

HCID 6881941-Hydroxy-6-(trifluoromethyl)benzotriazole수율 89.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The title compound is prepared according to the procedure described by K. Takeda [J. Org. Chem., 50, 273, (1985)]. A mixture of 4-chloro-3-nitro-α,α,α-trifluorotoluene (50.0 g, 0.22 moles) and hydrazine hydrate (33.0, 0.33 moles) in absolute ethanol (75 ml) is refluxed for 24 h. After removal of the solvent under reduced pressure, the residue is dissolved in 10% aqueous sodium carbonate solution. The solution is washed with ether to remove the starting material and acidified with concentrated HCl to precipitate the product, which is washed with water and dried to obtain 40.0 g of the title compound. This product is recrystallized from ether.

후처리

  1. customThe title compound is prepared
  2. temperatureis refluxed for 24 h
  3. customAfter removal of the solvent under reduced pressure
  4. dissolutionthe residue is dissolved in 10% aqueous sodium carbonate solution
  5. washThe solution is washed with ether
  6. customto remove the starting material
  7. customto precipitate the product, which
  8. washis washed with water
  9. customdried

출처 및 근거

ORD 기록
ord-868789ba44d24a379570d31b85128dc2
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094872B2

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