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Acetic Acid → 3-Bromo-4-(trifluoromethyl)benzoic acid

HRID 1475772
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HRID 1475772 반응식
N[C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[C:11]([F:14])([F:13])[F:12])[C:5]([OH:7])=[O:6].C(O)(=O)C.[BrH:19].N([O-])=O.[Na+]>O>[Br:19][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[C:11]([F:14])([F:13])[F:12])[C:5]([OH:7])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 260Hydrogen Bromide2회HCID 6426513-Amino-4-(trifluoromethyl)benzoic acidHCID 23668193Sodium Nitrite

생성물 1

HCID 223375703-Bromo-4-(trifluoromethyl)benzoic acid

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

5.0 g of 3-amino-4-trifluoromethyl-benzoic acid were dissolved using 50 ml of acetic acid. Then, 50 g of ice and 50 ml of a saturated aqueous HBr-solution were added and a solution of 2.0 g NaNO2 in 10 ml of water was added dropwise at 0° C. The reaction mixture was then stirred at room temperature for 10 minutes. Then, the reaction mixture was added dropwise to a suspension of 7.0 g CuBr and 10.9 g CuBr2 in 100 ml of a half-concentrated aqueous solution of HBr. The resulting mixture was then stirred for 2 h at room temperature, then diluted using 21 of water, stirred for 1 h and finally the precipitate was isolated by filtration. The precipitate was dried in vacuo to yield 5.2 g of the title compound that was used without further purification.

후처리

  1. stirringThe resulting mixture was then stirred for 2 h at room temperature
  2. additiondiluted
  3. stirringstirred for 1 h
  4. customfinally the precipitate was isolated by filtration
  5. customThe precipitate was dried in vacuo

출처 및 근거

ORD 기록
ord-5b18156a578b4db88242592fc18235e3
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09018383B2

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