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Carbon Tetrachloride → HCID 14999113, 화합물

HRID 1493240
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HRID 1493240 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O[CH2:21][CH2:22][N:23]1[C:27](=[O:28])[CH:26]([CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37])[S:25][CH:24]1[C:38]1[CH:39]=[N:40][CH:41]=[CH:42][CH:43]=1.C(Cl)(Cl)(Cl)[Cl:45]>>[Cl:45][CH2:21][CH2:22][N:23]1[C:27](=[O:28])[CH:26]([CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37])[S:25][CH:24]1[C:38]1[CH:39]=[N:40][CH:41]=[CH:42][CH:43]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 14999112HCID 14999112, 화합물

생성물 1

HCID 14999113HCID 14999113, 화합물수율 80%

실험 절차

Triphenylphosphine (3.44 g, 13 mmol) was added to a mixture of 3-(2-hydroxyethyl)-5-(n-nonyl)-2-(3-pyridyl)thiazolidin-4-one (3.49 g, 10 mmol) and carbon tetrachloride (20 ml) with stirring at room temperature. Then the mixture was refluxed with stirring for 2.5 hours. The product mixture was cooled and filtered to remove the formed crystals. The filtrate was concentrated and chromatographed, giving the cis-isomer (0.55 g) and trans-isomer (1.46 g) of the title compound and a mixture of two isomers (0.94 g) (total 2.95 g, 80% yield).

후처리

  1. temperatureThen the mixture was refluxed
  2. stirringwith stirring for 2.5 hours
  3. temperatureThe product mixture was cooled
  4. filtrationfiltered
  5. customto remove the formed crystals
  6. concentrationThe filtrate was concentrated
  7. customchromatographed

출처 및 근거

ORD 기록
ord-70bba3a3c6a6418886b589dd56d47aa5
출처 데이터셋
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05021435

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