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P-Cresol → HCID 9881592, 화합물

HRID 1586005
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HRID 1586005 반응식
[Na].Cl[C:3]1[N:4]=[N:5][C:6]([S:9][CH2:10][CH:11]=[CH2:12])=[CH:7][CH:8]=1.[CH:13]1[C:18]([OH:19])=[CH:17][CH:16]=[C:15]([CH3:20])[CH:14]=1>>[CH3:20][C:15]1[CH:14]=[CH:13][C:18]([O:19][C:3]2[N:4]=[N:5][C:6]([S:9][CH2:10][CH:11]=[CH2:12])=[CH:7][CH:8]=2)=[CH:17][CH:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 2879P-CresolHCID 5360545SodiumHCID 212176673-Chloro-6-[(prop-2-en-1-yl)sulfanyl]pyridazine

생성물 1

HCID 9881592HCID 9881592, 화합물

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온도
100 °C

실험 절차

0.23 g(0.01 mol) of metallic sodium was dissolved in 30 ml of dry p-cresol. To the resulting solution was added 1.87 g(0.01 mol) of 3-chloro-6-allylthiopyridazine and then the reaction solution was stirred for 5 hours at 100±5° C. After the reaction was allowed to stop, the reaction solution was cooled and adjusted to alkaline (pH 14) with 150 ml of 2N--NaOH, thereby precipitating the crystals. The precipitated crystal was extracted with diethyl ether, washed twice with purified water, dried over anhydrous magnesium sulfate and then concentrated to remove diethyl ether. The resulting oily residue was slowly cooled to obtain the title compound as a pale white amorphous crystal.

후처리

  1. temperaturethe reaction solution was cooled
  2. customNaOH, thereby precipitating the crystals
  3. extractionThe precipitated crystal was extracted with diethyl ether
  4. washwashed twice with purified water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customto remove diethyl ether
  8. temperatureThe resulting oily residue was slowly cooled

출처 및 근거

ORD 기록
ord-7571f0ff64d54e3695bb6bbff0bcc8a2
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05942511

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