Sodium Iodide → Dimethyl acetyl phosphate

HRID 1741762노트

반응식

HRID 1741762 반응식
[P:1]([O-:7])([O:5][CH3:6])([O:3][CH3:4])=[O:2].[Na+].P(OC)(OC)(OC)=O.[I-].[Na+].[C:19](Cl)(=[O:21])[CH3:20]>O1CCCC1>[P:1]([O:7][C:19](=[O:21])[CH3:20])([O:5][CH3:6])([O:3][CH3:4])=[O:2]

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 6367Acetyl chlorideHCID 10541Trimethyl PhosphateHCID 23663684Sodium dimethyl phosphate

생성물 1

HCID 14665382Dimethyl acetyl phosphate수율 80%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A suspension of sodium dimethyl phosphate (14.8 g, 0.1 mmol, from trimethyl phosphate and sodium iodide and acetyl chloride (7.8 g, 0.1 mmol) in dry tetrahydrofuran (80 mn) was stirred for two days at room temperature in a flask fitted with a drying tube. The reaction solution was filtered and the tetrahydrofuran was removed under reduced pressure. The resulting colorless liquid was Kugelrohr-distilled (Aldrich Kugelrohr apparatus, 55°-60° C. 0.30 torr) to give 14.2 g (80%) of dimethyl acetyl phosphate.

후처리

  1. customfitted with a drying tube
  2. filtrationThe reaction solution was filtered
  3. customthe tetrahydrofuran was removed under reduced pressure
  4. distillationThe resulting colorless liquid was Kugelrohr-distilled (Aldrich Kugelrohr apparatus, 55°-60° C. 0.30 torr)

출처 및 근거

ORD 기록
ord-066fbcfb554c4382980d8c292f3fdf83
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05334707

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