Methanol → HCID 23695619, 화합물

HRID 1089362노트

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HRID 1089362 반응식
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]

참가 물질

5

반응물 3

HCID 887MethanolHCID 165815Lithium sulfate monohydrateHCID 131716683HCID 131716683, 화합물

생성물 1

HCID 23695619HCID 23695619, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-273d87ae76f545d39d7d1e9d5a0ef6d1
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04965404

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