Water → Borane, tris(pentafluorophenyl)-, trihydrate

HRID 1977448

Reaktionsgleichung

Reaktionsgleichung von HRID 1977448
[B:1]([C:24]1[C:33]([F:34])=[C:31]([F:32])[C:29]([F:30])=[C:27]([F:28])[C:25]=1[F:26])([C:13]1[C:22]([F:23])=[C:20]([F:21])[C:18]([F:19])=[C:16]([F:17])[C:14]=1[F:15])[C:2]1[C:11]([F:12])=[C:9]([F:10])[C:7]([F:8])=[C:5]([F:6])[C:3]=1[F:4].C1CCCCC1.[OH2:41]>>[B:1]([C:13]1[C:22]([F:23])=[C:20]([F:21])[C:18]([F:19])=[C:16]([F:17])[C:14]=1[F:15])([C:24]1[C:33]([F:34])=[C:31]([F:32])[C:29]([F:30])=[C:27]([F:28])[C:25]=1[F:26])[C:2]1[C:3]([F:4])=[C:5]([F:6])[C:7]([F:8])=[C:9]([F:10])[C:11]=1[F:12].[OH2:41].[OH2:41].[OH2:41]

Komponenten

4

Edukt 3

HCID 962Water2×HCID 8078CyclohexaneHCID 582056Tris(pentafluorophenyl)borane

Produkt 1

HCID 11261567Borane, tris(pentafluorophenyl)-, trihydrate

Versuchsvorschrift

The synthesis of reported here is based on a prior publication (see U.S. Pat. No. 5,296,433, 1994). A 3.15 wt % solution of B(C6F5)3 in Isopar®E (50 ml, 2.22 mmol) was placed in a 200 ml Kjeldahl flask equipped with a magnetic stir bar. Approximately 50 ml of cyclohexane was added to this solution followed by 3 equiv of deoxygenated, demineralized water (0.120 ml, 6.67 mmol), which resulted in precipitation of a white, microcrystalline solid. The slurry was stirred for 30 m, the solvent was decanted, and the resulting solid was dried in vacuo. Yield, 0.826 g (66%). 19F NMR (C6D6): −134.7 (apparent d, 2F), −154.7 (apparent t, 1F), −162.6 (apparent t, 2F). FI-MS: m/z 512 [M+], evidently loss of water occurred in mass spectrometer. IR (Nujol): 3666 m, 3597 m, 3499 m, 2950 sh, 2920 s, 1647 m, 1602 m, 1520 s, 1468 s, 1379 m, 1288 m, 1111 m, 1098 m, 969 s, 859 w, 797 w, 771 w, 676 w, 614 w.

Aufarbeitung

  1. customThe synthesis
  2. customequipped with a magnetic stir bar
  3. customof deoxygenated
  4. customthe solvent was decanted
  5. customthe resulting solid was dried in vacuo
  6. customYield
  7. custom3666 m, 3597 m, 3499 m, 2950 sh, 2920 s, 1647 m, 1602 m, 1520 s, 1468 s, 1379 m, 1288 m, 1111 m, 1098 m, 969 s, 859 w, 797 w, 771 w, 676 w, 614 w

Quellen und Nachweise

ORD-Eintrag
ord-9855567df76749c9b30acc919fc6fc1b
Quelldatensatz
uspto-grants-2001_05
Patentnummer
US06232417B1

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