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4-trimethylsilylaniline → HCID 17912568, 화합물

HRID 963547
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HRID 963547 반응식
[F:1][C:2]([F:10])=[CH:3][CH2:4][CH2:5][CH2:6][C:7](Cl)=[O:8].[CH3:11][Si:12]([CH3:21])([CH3:20])[C:13]1[CH:19]=[CH:18][C:16]([NH2:17])=[CH:15][CH:14]=1>O1CCCC1>[CH3:11][Si:12]([CH3:21])([CH3:20])[C:13]1[CH:19]=[CH:18][C:16]([NH:17][C:7](=[O:8])[CH2:6][CH2:5][CH2:4][CH:3]=[C:2]([F:10])[F:1])=[CH:15][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 100349574-trimethylsilylanilineHCID 197938396,6-Difluorohex-5-enoic acid chloride

생성물 1

HCID 17912568HCID 17912568, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

With cooling at 10°, 1.0 g of 6,6-difluorohex-5-enoic acid chloride is added to 1.0 g of 4-trimethylsilylaniline, 0.73 g of trithylamine and 10 mg of 4-N-pyrrolidinopyridine in 25 ml of tetrahydrofuran. The mixture is stirred for 2 hours at room temperature and then concentrated by evaporation in vacuo. The residue is taken up in toluene, the toluene phase is washed with water, dried over sodium sulfate and concentrated to dryness by evaporation. The residue is taken up in hexane:ethyl acetate (9:1) and filtered over silica gel. Evaporation of the filtrate yields the title compound having a melting point of 50°-51° (compound no. 1-1).

후처리

  1. temperatureWith cooling at 10°
  2. concentrationconcentrated by evaporation in vacuo
  3. washthe toluene phase is washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to dryness by evaporation
  6. filtrationfiltered over silica gel
  7. customEvaporation of the filtrate

출처 및 근거

ORD 기록
ord-3761c0dc94484fe6a08de3592d205b23
출처 데이터셋
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05763481

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