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Dimethylformamide → HCID 58788081, 화합물

HRID 2055760
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HRID 2055760 반응식
CN([CH:4]=[O:5])C.O[C:7]1[CH:8]=[C:9]([CH:14]=[C:15]([OH:17])[CH:16]=1)[C:10]([O:12][CH3:13])=[O:11].C(=O)([O-])[O-].[K+].[K+].Br[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36]>O>[CH2:25]([O:17][C:15]1[CH:14]=[C:9]([CH:8]=[C:7]([O:5][CH2:4][CH2:35][CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH3:25])[CH:16]=1)[C:10]([O:12][CH3:13])=[O:11])[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228Dimethylformamide2회HCID 89191-BromododecaneHCID 11430Potassium CarbonateHCID 75076Methyl 3,5-Dihydroxybenzoate

생성물 1

HCID 58788081HCID 58788081, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

In a 1 L RBF containing a stir bar and DMF (100 mL); methyl 3,5-dihydroxylbenzoate (20 g, 0.1190 M), potassium carbonate (49.34 g, 0.3570 M), 1-bromododecane (57.2 mL, 0.2380 M) and DMF (100 mL) were added. The reaction mixture was covered with a septum and stirred overnight. By the end of the reaction period (15 hours), the reaction mixture had turned from a pale yellow suspension to a solid dark green suspension. Heat was applied to the RBF until the reaction mixture became fluid. The dark green mixture was then added to 1 L of distilled water and ice, and copious precipitation occurred immediately. The precipitate was isolated by vacuum filtration. The precipitate was recrystallized from hot ethanol (1 L). To increase the product yield, the solution was left to stand at room temperature overnight. The crystals were vacuum filtered and the crystals air-dried yielding 58.5 g or 96.7%. The NMR characterization data for the derivative is as follows. 1H NMR (300 MHz, CDCl3): 0.87 (t, J=6.6, 6H, CH2CH3), 1.15-1.6 (m, 28H, CH2(CH2)6), 1.76 (p, J=8.0, 8H, OCH2CH2), 3.89 (s, 3H, OCH3), 3.95 (t, J=6.6, 4H, OCH2CH2), 6.62 (t, J=2.5, 1H, ArH), 7.15 (d, J=2.5, 2H, ArH).

후처리

  1. additionIn a 1 L RBF containing a stir bar
  2. customBy the end of the reaction period (15 hours)
  3. temperatureHeat
  4. customThe precipitate was isolated by vacuum filtration
  5. customThe precipitate was recrystallized from hot ethanol (1 L)
  6. temperatureTo increase the product
  7. customyield
  8. waitthe solution was left
  9. waitto stand at room temperature overnight
  10. filtrationfiltered
  11. customthe crystals air-dried
  12. customyielding 58.5 g or 96.7%

출처 및 근거

ORD 기록
ord-c5404a0b178f43f1843248f06cdbb96c
출처 데이터셋
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07332529B2

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