Dimethyl methylphosphonate → Antimony Pentachloride Dimethylmethylphosphonate

HRID 354618

반응식

HRID 354618 반응식
[Sb:1]([Cl:6])([Cl:5])([Cl:4])([Cl:3])[Cl:2].[CH3:7][O:8][P:9]([CH3:13])(=[O:12])[O:10][CH3:11]>C(Cl)Cl>[Sb:1]([Cl:6])([Cl:5])([Cl:4])([Cl:3])[Cl:2].[CH3:7][O:8][P:9]([CH3:13])(=[O:12])[O:10][CH3:11]

참가 물질

4

반응물 2

HCID 12958Dimethyl methylphosphonateHCID 24294Antimony pentachloride

생성물 1

HCID 131712430Antimony Pentachloride Dimethylmethylphosphonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

In a round bottom flask, under a nitrogen atmosphere, 7.61 g (0.0254 M) of antimony pentachloride was dissolved in 75 ml of methylene chloride. To this yellow solution was added dropwise with stirring a solution of 3.16 g (0.0254 M) of dimethylmethylphosphonate in 20 ml of methylene chloride. The addition was accomplished at a rate such that the exotherm did not become excessive, the temperature being kept below the reflux temperature of methylene chloride (cooling should not be required). By the end of the addition, the initial yellow color had dissipated. The reaction mixture was stirred at ambient temperature for one hour, after which time the solvent was removed by evaporation at reduced pressure. Th crystalline product was thoroughly dried in vacuo (0.1 mm Hg). Analysis calculated for C3H9Cl5O3PSb: % Cl=41.9, observed=42.0%. NMR (CDCl3, TMS): δ4.12 (d,6H,J=11.6 Hz), 2.08 (d,3H,J=17.6 Hz).

후처리

  1. additionTo this yellow solution was added dropwise
  2. additionThe addition
  3. temperaturecooling should not
  4. additionBy the end of the addition
  5. customafter which time the solvent was removed by evaporation at reduced pressure
  6. customTh crystalline product was thoroughly dried in vacuo (0.1 mm Hg)

출처 및 근거

ORD 기록
ord-1c0c547777654616b4886c030396308f
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04376063

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