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Aniline → HCID 18420339、化合物

HRID 990322
ノート
印刷プレビュー

反応式

HRID 990322 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 6115AnilineHCID 7918Acetic AnhydrideHCID 66019TetramethoxypropaneHCID 517045Sodium AcetateHCID 371329865756-50-5HCID 18420329HCID 18420329、化合物

生成物 1

HCID 18420339HCID 18420339、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1ee00b03bbbc4f4897adbbbe5e41c78d
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06458967B1

反応ノート

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