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Aniline → HCID 18420339, 화합물

HRID 990322
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HRID 990322 반응식
N[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CO[CH:10](OC)[CH2:11][CH:12](OC)OC.C([O-])(=O)C.[Na+].[NH3+]C1C=CC=CC=1.[F:31][P-:32]([F:37])([F:36])([F:35])([F:34])[F:33].C([C:41]1[CH:46]=[CH:45][C:44]([C:47]2[CH:52]=[C:51]([CH3:53])[CH:50]=[C:49](C3C=CC=CC=3)[S+:48]=2)=[CH:43][CH:42]=1)(C)C.C(OC(=O)C)(=O)C>C(O)(=O)C.O>[F:31][P-:32]([F:37])([F:36])([F:35])([F:34])[F:33].[CH:11]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:49]1[CH:50]=[C:51]([CH3:53])[CH:52]=[C:47]([C:44]2[CH:43]=[CH:42][CH:41]=[CH:46][CH:45]=2)[S+:48]=1)([CH3:12])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 6115AnilineHCID 7918Acetic AnhydrideHCID 66019TetramethoxypropaneHCID 517045Sodium AcetateHCID 371329865756-50-5HCID 18420329HCID 18420329, 화합물

생성물 1

HCID 18420339HCID 18420339, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 962Water용매

실험 절차

C45H41F6 PS2, FW=790.90 g/mol. Aniline (2.86 g, 30.0 mmol) and 1,1,3,3-tetramethoxypropane (1.99 g, 12.1) were dissolved in acetic acid (10 mL) and heated to 80 C for 15 minutes. The solution was removed from the heat and a 60% solution of hexafluorophosphoric acid (2 mL) was slowly added. The reaction mixture was then poured into water (200 mL) and the anilinium hexafluorophosphate salt of 1,1,3,3-tetramethoxypropane, a yellow solid, was collected. Sodium acetate (0.023 g, 0.24 mmol), anilinium salt (0.044 g, 0.12 mmol), and 2-(4-Isopropylphenyl)-6-(phenyl)-4-methylthiopyrylium hexafluorophosphate (0.108 g, 0.24 mmol) are combined in a flask containing acetic anhydride (0.6 mL) and acetic acid (0.6 mL). The reaction is heated to 95 C for 8 minutes. Once the reaction is complete, the reaction mixture is poured into water and the brown precipitate is filtered off. The precipitate is dissolved in acetonitrile and crystallized out with ether. The resulting red crystals are collected in 63% yield. Melting point 165-167° C.; 1H NMR (500 MHz, CD3CN, ppm) d 7.65 (t, 2H, J=19.4 Hz), 7.34 (d, 4H, J=7.33 Hz), 7.25 (s, 10H), 7.22 (d, 4H, J=6.6 Hz), 7.09 (d, 2H, J=7.7 Hz), 6.42 (t, 1H, J=12.1 Hz), 6.23 (d, 2H, J=13.6 Hz), 2.82 (m, 2H), 1.16 (d, 12H, 7.0 Hz); UV(DCM): max 893 nm (log e 312,000±17,000 M−1 cm−1).

후처리

  1. temperatureheated to 80 C for 15 minutes
  2. customThe solution was removed from the
  3. temperatureheat
  4. additiona 60% solution of hexafluorophosphoric acid (2 mL) was slowly added
  5. additionThe reaction mixture was then poured into water (200 mL)
  6. customthe anilinium hexafluorophosphate salt of 1,1,3,3-tetramethoxypropane, a yellow solid, was collected
  7. temperatureThe reaction is heated to 95 C for 8 minutes
  8. filtrationthe brown precipitate is filtered off
  9. dissolutionThe precipitate is dissolved in acetonitrile
  10. customcrystallized out with ether
  11. customThe resulting red crystals are collected in 63% yield

출처 및 근거

ORD 기록
ord-1ee00b03bbbc4f4897adbbbe5e41c78d
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06458967B1

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