Sodium Iodide → Dimethyl acetyl phosphate

HRID 1741762ノート

反応式

HRID 1741762 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 14665382Dimethyl acetyl phosphate収率 80%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-066fbcfb554c4382980d8c292f3fdf83
出典データセット
uspto-grants-1994_08
特許番号
US05334707

反応ノート

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