2,6-Lutidine → (Diethoxyphosphoryl)methyl trifluoromethanesulfonate

HRID 1807437ノート

反応式

HRID 1807437 の反応式
[CH2:1]([O:3][P:4]([CH2:9]CO)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].N1C(C)=CC=CC=1C.[F:20][C:21]([F:34])([F:33])[S:22]([O:25]S(C(F)(F)F)(=O)=O)(=[O:24])=[O:23]>ClCCl.C(OCC)C>[F:20][C:21]([F:34])([F:33])[S:22]([O:25][CH2:9][P:4]([O:3][CH2:1][CH3:2])([O:5][CH2:6][CH3:7])=[O:8])(=[O:24])=[O:23]

参加物

6

反応物 3

HCID 79372,6-LutidineHCID 67749Trifluoromethanesulfonic anhydrideHCID 312225Diethyl (2-hydroxyethyl)phosphonate

生成物 1

HCID 11833487(Diethoxyphosphoryl)methyl trifluoromethanesulfonate

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-50 °C

実験手順

5.01 ml diethyl-(hydroxyethyl)-phosphonate are dissolved in 50 ml dichloromethane, combined with 4.42 ml of 2,6-lutidine and cooled to −50° C. Then a solution of 6 ml trifluoromethanesulphonic acid anhydride in 10 ml dichloromethane is slowly added dropwise. The mixture is allowed to come up to 0° C. within 1.5 hours and then diluted with 300 ml of cold diethyl ether. The precipitated solids are filtered off and the filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution. After drying with sodium sulphate the solvents are eliminated in vacuo.

後処理

  1. filtrationThe precipitated solids are filtered off
  2. washthe filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution
  3. dry with materialAfter drying with sodium sulphate the solvents

出典と根拠

ORDレコード
ord-4ffe84da72c1410a808b28b05147dac5
出典データセット
uspto-grants-2013_01
特許番号
US08357689B2

反応ノート

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