Triethyl phosphite → Phosphonic acid, P,P'-(1,4-phenylenebis(methylene))bis-, P,P,P',P'-tetraethyl ester

HRID 2222748

反応式

HRID 2222748 の反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9]Br)=[CH:5][CH:4]=1.[P:11]([O:18][CH2:19][CH3:20])([O:15][CH2:16][CH3:17])[O:12]CC>>[C:6]1([CH2:9][P:11](=[O:12])([O:15][CH2:16][CH3:17])[O:18][CH2:19][CH3:20])[CH:7]=[CH:8][C:3]([CH2:2][P:11](=[O:12])([O:18][CH2:19][CH3:20])[O:15][CH2:16][CH3:17])=[CH:4][CH:5]=1

参加物

3

反応物 2

HCID 31215Triethyl phosphiteHCID 693351,4-Bis(bromomethyl)benzene

生成物 1

HCID 78303Phosphonic acid, P,P'-(1,4-phenylenebis(methylene))bis-, P,P,P',P'-tetraethyl ester収率 89.1%

反応条件

温度
130 °C

実験手順

α, α′-Dibromo-p-xylene (5.28 g, 20 mmol, 1 equiv.) and triethyl phosphite (10.3 mL, 60 mmol, 3 equiv.) were placed in a flask with a magnetic stirring bar. A distillation apparatus was attached to collect ethyl bromide formed along with the reaction. The mixture was immersed in an oil bath and heated to 130° C. for 2 h. After cooling down, white crystal crushed out and recrystalized from hexane to give the product (6.74 g, 89% yield). 1H NMR (CDCl3) δ7.24 (s, 4H), 4.00 (m, 8H), 3.12 (d, 4H, J=20.2 Hz), 1.23 (t, 12H, J=7.0 Hz).

後処理

  1. customto collect ethyl bromide
  2. customformed along with the reaction
  3. customThe mixture was immersed in an oil bath
  4. temperatureAfter cooling down
  5. customwhite crystal crushed out and
  6. customrecrystalized from hexane

出典と根拠

ORDレコード
ord-f43118ed414e415a8a83585a3fbbb3f5
出典データセット
uspto-grants-2008_05
特許番号
US07371887B2

関連ノート

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