Hydrochloric Acid → Dibutyl(1-hydroxy-1,3-dimethylbutyl)phosphonate

HRID 13742

反応式

HRID 13742 の反応式
Cl.[CH2:2]([O:6][P:7]([O-:13])[O:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH2:3][CH2:4][CH3:5].[CH2:14]([C:18]([CH3:20])=[O:19])[CH:15]([CH3:17])[CH3:16]>C(N(CC)CC)C.[Cl-].[Mg+2].[Cl-]>[CH2:9]([O:8][P:7]([C:18]([OH:19])([CH3:20])[CH2:14][CH:15]([CH3:17])[CH3:16])(=[O:13])[O:6][CH2:2][CH2:3][CH2:4][CH3:5])[CH2:10][CH2:11][CH3:12]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 7909Methyl Isobutyl KetoneHCID 23414612Dibutylphosphite

生成物 1

HCID 86241711Dibutyl(1-hydroxy-1,3-dimethylbutyl)phosphonate収率 92.3%

試薬・触媒・溶媒 2

HCID 8471Triethylamine触媒HCID 5360315Magnesium Chloride触媒

実験手順

Into a two-liter four-necked flask provided with a stirrer, a thermometer, dropping device, a hydrochloric-acid-recovering device and a condenser, 213.4 g (1.1 moles) of dibutylphosphite, 5.6 g (0.06 moles) of triethylamine and 1.05 g (0.011 moles) of magnesium chloride were fed. While stirring the resulting mixed solution at 25° C., 120.0 g (1.2 moles) of methyl isobutyl ketone (MIBK) was added thereto in 1 hour. The resulting mixed solution was further stirred for 1 hour at the same temperature (25° C.) to complete the reaction. Thereafter, the mixed solution was washed to remove the low-boiling point portions, as in (synthesis of raw material 2) of Example 1, and thus, the triethylamine and the magnesium chloride was removed from the mixed solution, to obtain 298.8 g of dibutyl(1-hydroxy-1,3-dimethylbutyl)phosphonate (raw material 3).

後処理

  1. customInto a two-liter four-necked flask provided with a stirrer
  2. additionmixed solution at 25° C.
  3. additionThe resulting mixed solution
  4. stirringwas further stirred for 1 hour at the same temperature (25° C.)
  5. customthe reaction
  6. washThereafter, the mixed solution was washed
  7. customto remove the low-boiling point portions
  8. customas in (synthesis of raw material 2) of Example 1
  9. customthus, the triethylamine and the magnesium chloride was removed from the mixed solution

出典と根拠

ORDレコード
ord-c4dbe71e53fe47f5aca8f35e02e13474
出典データセット
uspto-grants-2010_06
特許番号
US07728162B2

関連ノート

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