Water → Bis(pentafluorophenyl)borinic acid

HRID 1359537

反応式

HRID 1359537 の反応式
[F:1][C:2]1[C:7]([B:8](C2C(F)=C(F)C(F)=C(F)C=2F)[C:9]2[C:14]([F:15])=[C:13]([F:16])[C:12]([F:17])=[C:11]([F:18])[C:10]=2[F:19])=[C:6]([F:31])[C:5]([F:32])=[C:4]([F:33])[C:3]=1[F:34].[OH2:35]>CCCCCCC.C1(C)C=CC=CC=1>[F:1][C:2]1[C:7]([B:8]([C:9]2[C:14]([F:15])=[C:13]([F:16])[C:12]([F:17])=[C:11]([F:18])[C:10]=2[F:19])[OH:35])=[C:6]([F:31])[C:5]([F:32])=[C:4]([F:33])[C:3]=1[F:34]

参加物

5

反応物 2

HCID 962WaterHCID 582056Tris(pentafluorophenyl)borane

生成物 1

HCID 9841889Bis(pentafluorophenyl)borinic acid

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8900Heptane溶媒

反応条件

温度
0 °C

実験手順

20 g (39 mmol) of tris(pentafluorophenyl)borane are suspended in 150 ml of heptane and, under reflux, a solution of 1.8 ml (97.5 mmol) of water in 40 ml of toluene is then added over a period of 30 minutes. The mixture is subsequently stirred for another five hours under reflux. The solution is subsequently cooled to 0° C. Over a period of 30 minutes, the product precipitates as a white solid. The product is isolated and washed three times with 50 ml each time of pentane and subsequently dried in an oil pump vacuum. This gives 11.5 g (80%) of colorless bis(pentafluorophenyl)hydroxyborane. The boroxin content is 10%. 1H-NMR(C6D6, 400 MHz): −133.1 (m, 4 F, o-B(C6F5)2), −147.9 (m, 2 F, p-B(C6F5)2), −161.1 (m, 4 F, m-B(C6F5)2) ppm.

後処理

  1. temperatureunder reflux
  2. temperatureunder reflux
  3. waitOver a period of 30 minutes
  4. customthe product precipitates as a white solid
  5. customThe product is isolated
  6. washwashed three times with 50 ml each time of pentane
  7. customsubsequently dried in an oil pump vacuum

出典と根拠

ORDレコード
ord-fb6d8420c5bc45c7b43f42e3ab89169b
出典データセット
uspto-grants-2003_07
特許番号
US06600066B1

関連ノート

読み込み中…