Oxalyl chloride → HCID 21054123、化合物

HRID 2354489ノート

反応式

HRID 2354489 の反応式
[CH2:1]([O:3][P:4]([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])(=O)[O:5]CC)[CH3:2].C(Cl)(=O)C([Cl:22])=O>C(OCC)C>[CH2:9]([P:4]([Cl:22])(=[O:5])[O:3][CH2:1][CH3:2])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

参加物

4

反応物 2

HCID 65578Oxalyl chlorideHCID 2773697Diethyl decylphosphonate

生成物 1

HCID 21054123HCID 21054123、化合物収率 73%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
-20 °C

実験手順

To a 500 mL round bottomed flask containing n-decylphosphonic acid diethyl ester, 22 g (79.0 mmol) was added to 100 mL of diethylether. This solution was stirred and cooled to −20° C. using an ice/salt water bath. Oxalyl Chloride (20.06 g, 158 mmol) was added in small portions over 45 minutes while maintaining the temperature at −20° C. The reaction mixture was then allowed to warm to room temperature and stirred for 24 hours. The solvent was removed by rotary evaporation to give a viscous liquid. The liquid was purified by vacuum distillation (boiling point: 126° C. at 0.4 mmHg) to give 15.5 g (73% yield) of the desired product. 1H NMR (400 MHz CDCl3): δ 4.2 (m, 2H), 2.0 (m, 2H), 1.6 (m, 2H), 1.2 (m, 17H), 0.75 (t, 3H).

後処理

  1. temperaturewhile maintaining the temperature at −20° C
  2. temperatureto warm to room temperature
  3. stirringstirred for 24 hours
  4. customThe solvent was removed by rotary evaporation
  5. customto give a viscous liquid
  6. distillationThe liquid was purified by vacuum distillation (boiling point: 126° C. at 0.4 mmHg)

出典と根拠

ORDレコード
ord-78f8cefa24474132824a1320633dcd3e
出典データセット
uspto-grants-2010_07
特許番号
US07754200B2

反応ノート

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