Methanol → HCID 23695619、化合物

HRID 1089362ノート

反応式

HRID 1089362 の反応式
CO.O.O.[C:5]1([P:11]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([S:24]([O-:27])(=[O:26])=[O:25])[CH:19]=2)[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[K+].O.S([O-])([O-])(=O)=O.[Li+:35].[Li+]>C(O)(C)C>[C:5]1([P:11]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([S:24]([O-:27])(=[O:26])=[O:25])[CH:19]=2)[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1.[Li+:35]

参加物

5

反応物 3

HCID 887MethanolHCID 165815Lithium sulfate monohydrateHCID 131716683HCID 131716683、化合物

生成物 1

HCID 23695619HCID 23695619、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A one-liter three-necked flask equipped with stirrer, reflux condenser and nitrogen gas inlet and outlet was charged under nitrogen atmosphere with 250 ml of methanol, 250 ml of isopropanol and 157 g of potassium diphenylphosphinobenzene-m-monosulfonate dihydrate obtained in Reference Example 2, thereafter 48 g of lithium sulfate monohydrate. The mixture was refluxed for 6 hours with stirring. After completion of the reaction, inorganic salts were removed by filtration. To the obtained mother liquor was added 250 ml of toluene, thereafter methanol and isopropanol were distilled off to replace the solvent with toluene. Precipitated crystalline of lithium diphenylphosphinobenzene-m-monosulfonate was isolated by filtration. The collected lithium diphenylphosphinobenzene-m-monosulfonate was dried at 150° C. under reduced pressure of 5 mmHg for 4 hours to give 128 g lithium diphenylphosphinobenzene-m-monosulfonate. It was revealed by the analyses of elemental analysis, ion chromatography, liquid chromatography, etc. that the obtained lithium diphenylphosphinobenzene-m-monosulfonate had a purity of 100%.

後処理

  1. customA one-liter three-necked flask equipped with stirrer
  2. temperaturereflux condenser and nitrogen gas inlet and outlet
  3. customobtained in Reference Example 2
  4. temperatureThe mixture was refluxed for 6 hours
  5. customAfter completion of the reaction, inorganic salts
  6. customwere removed by filtration
  7. additionTo the obtained mother liquor was added 250 ml of toluene
  8. distillationmethanol and isopropanol were distilled off

出典と根拠

ORDレコード
ord-273d87ae76f545d39d7d1e9d5a0ef6d1
出典データセット
uspto-grants-1990_10
特許番号
US04965404

反応ノート

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