Triisopropyl phosphite → Diisopropyl phosphite

HRID 414906

反応式

HRID 414906 の反応式
C(OCCOCCl)(=O)C.[CH:10]([O:13][P:14]([O:19]C(C)C)[O:15][CH:16]([CH3:18])[CH3:17])([CH3:12])[CH3:11]>>[PH:14](=[O:19])([O:15][CH:16]([CH3:18])[CH3:17])[O:13][CH:10]([CH3:12])[CH3:11]

参加物

3

反応物 2

HCID 8304Triisopropyl phosphiteHCID 10034810Acetic acid 2-chloromethoxy-ethyl ester

生成物 1

HCID 3072Diisopropyl phosphite収率 47%

反応条件

温度
125 °C

実験手順

A 500 mL three-neck flask was charged with the crude chloromethylether 1 (317 g, 2.00 mol). Triisopropylphosphite (494 mL) was added dropwise through an additional funnel while heating in a 125° C. oil bath and stirring vigorously. Collect 2-chloropropane distillate via short-path head in a dry ice cooled receiver, argon blanket, collected 140 g distillate (theoretical 157 g). Phosphite blanched reaction to yellow, continue heating another 2 h at 125° C. oil bath, then arrange for vacuum distillation using a vacuum pump. Distilled a yellow front cut (140 g, head to 135° C., bottom to 190° C.), then changed to clean receiver. Main fraction was collected at head temperature of 178-187° C. (mostly 185-187° C.) with vacuum unknown at bath temperature of 222-228° C. 258 g of the product 2 was given (47% yield from 1,3-dioxolane).

後処理

  1. distillationCollect 2-chloropropane distillate via short-path head in a dry ice cooled receiver, argon blanket, collected 140 g distillate (theoretical 157 g)
  2. customreaction to yellow,
  3. temperaturecontinue heating another 2 h at 125° C. oil bath
  4. distillationarrange for vacuum distillation
  5. distillationDistilled a yellow front cut (140 g, head to 135° C., bottom to 190° C.)
  6. customMain fraction was collected at head temperature of 178-187° C. (mostly 185-187° C.) with vacuum unknown at bath temperature of 222-228° C

出典と根拠

ORDレコード
ord-a26f559d1f7e48569a465696f70f09e1
出典データセット
uspto-grants-2012_01
特許番号
US08088754B2

関連ノート

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