Water → Borane, tris(pentafluorophenyl)-, trihydrate

HRID 1977448

반응식

HRID 1977448 반응식
[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]

참가 물질

4

반응물 3

HCID 962Water2회HCID 8078CyclohexaneHCID 582056Tris(pentafluorophenyl)borane

생성물 1

HCID 11261567Borane, tris(pentafluorophenyl)-, trihydrate

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9855567df76749c9b30acc919fc6fc1b
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232417B1

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