Triethyl phosphite → HCID 23169886、化合物

HRID 374235

反応式

HRID 374235 の反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][C:12]([CH2:15]Br)=[CH:11][CH:10]=2)=[CH:5][CH:4]=1.C([O:19][P:20]([O:24]CC)[O:21]CC)C>>[P:20]([CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][C:12]([CH2:15][P:20]([OH:24])([OH:21])=[O:19])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1)([OH:24])([OH:21])=[O:19]

参加物

3

反応物 2

HCID 31215Triethyl phosphiteHCID 6212384,4'-Bis(bromomethyl)biphenyl

生成物 1

HCID 23169886HCID 23169886、化合物収率 123.1%

反応条件

温度
140 °C

実験手順

16.97 g (49.9 mmoles) of 4,4'-bis (bromomethyl) biphenyl and 52.04 ml (299.4 mmoles) of triethyl-phosphite are placed in a 250 ml flask which has a cooler and oil heating bath. The mixture is heated to 140° C. under magnetic agitation for 5 hours. On completion the excess triethyl-phosphite is separated by distillation and the white solid residue, redissolved in 50 ml of ethanol, is evaporated to dryness under vacuum, this operation being repeated twice. The residue is dissolved in 30 ml of ethanol and poured slowly into a beaker containing water and ice. The precipitate obtained is filtered on porous septum G3, washed with iced water (1 l) and under vacuum dried in an oven at 40° C., obtaining 21.02 g of 4,4'-bis (phosphonomethyl) biphenyl acid tetra-ethyl ester with a molar yield of 92.8%.

後処理

  1. temperatureheating bath
  2. customOn completion the excess triethyl-phosphite is separated by distillation
  3. dissolutionthe white solid residue, redissolved in 50 ml of ethanol
  4. customis evaporated to dryness under vacuum
  5. dissolutionThe residue is dissolved in 30 ml of ethanol
  6. additionpoured slowly into a beaker
  7. additioncontaining water and ice
  8. customThe precipitate obtained
  9. filtrationis filtered on porous septum G3
  10. washwashed with iced water (1 l) and under vacuum
  11. customdried in an oven at 40° C.

出典と根拠

ORDレコード
ord-5d4ff08f32d24961b132c431c0ff8eff
出典データセット
uspto-grants-1992_11
特許番号
US05166380

関連ノート

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