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N-bromobutanimide → 3'-Bromo-4'-hydroxy-5'-(trifluoromethyl)acetophenone

HRID 249723
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인쇄 미리보기

반응식

HRID 249723 반응식
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([C:11]([F:14])([F:13])[F:12])[CH:5]=1)=[O:3].[Br:15]N1C(=O)CCC1=O>C(#N)C>[Br:15][C:8]1[CH:9]=[C:4]([C:2](=[O:3])[CH3:1])[CH:5]=[C:6]([C:11]([F:12])([F:13])[F:14])[C:7]=1[OH:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 27751094'-Hydroxy-3'-(trifluoromethyl)acetophenone

생성물 1

HCID 580857003'-Bromo-4'-hydroxy-5'-(trifluoromethyl)acetophenone

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

4-Hydroxy-3-(trifluoromethyl)acetophenone (4 g) was initially introduced in acetonitrile (150 ml) and N-bromosuccinimide (4.5 g, dissolved in 100 ml acetonitrile) was added dropwise at −10° C. After addition was complete, the cooling bath was removed and the mixture was stirred for 5 h. After standing overnight, the volume of solvent was reduced to a quarter and the residue was treated with n-heptane/water. After separating off the organic phase, this was washed once with 5% strength sodium thiosulfate solution and once with water. The precipitate formed in the course of this (6.9 g) was filtered off with suction and directly reacted further in the next stage.

후처리

  1. additionAfter addition
  2. customthe cooling bath was removed
  3. waitAfter standing overnight
  4. additionthe residue was treated with n-heptane/water
  5. customAfter separating off the organic phase
  6. washthis was washed once with 5% strength sodium thiosulfate solution and once with water
  7. customThe precipitate formed in the course of this (6.9 g)
  8. filtrationwas filtered off with suction
  9. customdirectly reacted further in the next stage

출처 및 근거

ORD 기록
ord-0e04d23518e74dbda8e65ced2c99f3ff
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07863269B2

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