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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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p-Toluenesulfonic acid → HCID 22025506, 화합물

HRID 1792933
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HRID 1792933 반응식
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]2[C:10](=[O:11])[O:9][C:7](=O)[C:6]2=[CH:12][CH:13]=1.[CH2:16]([NH2:20])[CH:17]([CH3:19])[CH3:18].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[F:14][C:2]([F:1])([F:15])[C:3]1[CH:4]=[C:5]2[C:10](=[O:11])[N:20]([CH2:16][CH:17]([CH3:19])[CH3:18])[C:7](=[O:9])[C:6]2=[CH:12][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 6558IsobutylamineHCID 127177895-(Trifluoromethyl)isobenzofuran-1,3-dione

생성물 1

HCID 22025506HCID 22025506, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
140 °C

실험 절차

4-Trifluoromethyl-N-isobutylphthalimide is prepared as described in Example 2, starting with 14.8 g of 4-trifluoromethylphthalic anhydride, 7.2 cm3 of isobutylamine and a catalytic amount of para-toluenesulfonic acid in 160 cm3 of toluene. The reaction mixture is heated at a temperature in the region of 140° C. for 5 hours and is then cooled to a temperature in the region of 20° C. The reaction mixture is concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C. and the residue is taken up in 250 cm3 of ethyl acetate and 200 cm3 of saturated aqueous sodium hydrogen carbonate solution. The aqueous phase is separated out after settling has taken place and then extracted twice with 250 cm3 of ethyl acetate. The organic extracts are combined, washed with saturated brine, dried over magnesium sulfate, filtered and then concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C. 14.9 g of 4-trifluoromethyl-N-isobutylphthalimide are thus obtained in the form of a yellow powder (Rf=0.59, thin layer chromatography on silica gel, eluent: cyclohexane/ethyl acetate (75/25 by volume)).

후처리

  1. custom4-Trifluoromethyl-N-isobutylphthalimide is prepared
  2. temperatureis then cooled to a temperature in the region of 20° C
  3. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C.
  4. customThe aqueous phase is separated out after settling
  5. extractionextracted twice with 250 cm3 of ethyl acetate
  6. washwashed with saturated brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C

출처 및 근거

ORD 기록
ord-bc678ceaffb94426a0467a40e180f547
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07078428B2

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