Hydrochloric Acid → HCID 86738481、化合物

HRID 1759164ノート

反応式

HRID 1759164 の反応式
[CH3:1][O:2][C:3]([P:7]([CH3:11])(=[O:10])[O:8]C)([O:5][CH3:6])[CH3:4].Cl.[OH-].[Na+:14]>>[CH3:1][O:2][C:3]([P:7]([CH3:11])(=[O:8])[O-:10])([O:5][CH3:6])[CH3:4].[Na+:14]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 54446102Methyl (1,1-dimethoxyethyl)methylphosphinate

生成物 1

HCID 86738481HCID 86738481、化合物

実験手順

The phosphinate ester product of Example 16 (220 g) was refluxed 2 hr with aqueous sodium hydroxide (2 N: 660 ml). The cooled solution was taken to pH 7.0 with conc. hydrochloric acid, evaporated in vacuo and the solid residue was triturated with methanol and insoluble material filtered off. The filtrate was again evaporated to dryness, the residue triturated with methanol and further insoluble material filtered off. The filtrate was finally evaporated to dryness, triturated with acetone and filtered to give the title compound (2.9 g) mp 258°-262° C., identical (ir nmr) with the product from Example 17.

後処理

  1. customevaporated in vacuo
  2. customthe solid residue was triturated with methanol and insoluble material
  3. filtrationfiltered off
  4. customThe filtrate was again evaporated to dryness
  5. customthe residue triturated with methanol and further insoluble material
  6. filtrationfiltered off
  7. customThe filtrate was finally evaporated to dryness
  8. customtriturated with acetone
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-9cf1218397fa40f99dfc1368acc821ef
出典データセット
uspto-grants-1982_07
特許番号
US04339443

反応ノート

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