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Triethylamine → HCID 22708283, 화합물

HRID 353191
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HRID 353191 반응식
[CH:1]([C:4]1[CH:10]=[CH:9][C:7]([NH2:8])=[C:6]([C:11]([F:14])([F:13])[F:12])[CH:5]=1)([CH3:3])[CH3:2].C(N(CC)CC)C.[Br:22][CH2:23][C:24](Br)=[O:25]>ClCCl>[Br:22][CH2:23][C:24]([NH:8][C:7]1[CH:9]=[CH:10][C:4]([CH:1]([CH3:3])[CH3:2])=[CH:5][C:6]=1[C:11]([F:12])([F:13])[F:14])=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 61147Bromoacetyl bromideHCID 27752232-Amino-5-isopropylbenzotrifluoride

생성물 1

HCID 22708283HCID 22708283, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

50 g (246.06 mmol) of 4-isopropyl-2-(trifluoromethyl)aniline and 27.39 g (270.66 mmol) of triethylamine are initially charged in 1000 ml of dichloromethane. At 0°-5° C., 54.63 g (270.66 mmol) of bromoacetyl bromide, dissolved in 200 ml of dichloromethane, are added dropwise. The mixture is stirred at room temperature for 20 hours. The reaction mixture is then extracted successively with water, 1 N hydrochloric acid, water, saturated sodium bicarbonate solution and water. The organic phase is dried over sodium sulphate and the solvent is removed under reduced pressure. The residue is purified chromatographically. The product is recrystallized from cyclohexane/n-pentane, filtered off with suction and dried under reduced pressure at 40° C. for 20 hours. This gives 32.45 g (41% of theory) of the title compound.

후처리

  1. additionare added dropwise
  2. extractionThe reaction mixture is then extracted successively with water, 1 N hydrochloric acid, water, saturated sodium bicarbonate solution and water
  3. dry with materialThe organic phase is dried over sodium sulphate
  4. customthe solvent is removed under reduced pressure
  5. customThe residue is purified chromatographically
  6. customThe product is recrystallized from cyclohexane/n-pentane
  7. filtrationfiltered off with suction
  8. customdried under reduced pressure at 40° C. for 20 hours

출처 및 근거

ORD 기록
ord-9b1885902ddf49559ec173f9162ec972
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06750236B2

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