Benzoic Acid → Dipropylene Glycol Monomethyl Ether Benzoate

HRID 1709713

反応式

HRID 1709713 の反応式
[CH3:1][O:2][CH:3]([CH2:5][O:6][CH:7]([CH2:9][OH:10])[CH3:8])[CH3:4].[C:11](O)(=[O:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C1(C)C=CC=CC=1>C(=O)([O-])[O-].[Zr+4].C(=O)([O-])[O-].O>[C:11]([O:10][CH2:9][CH:7]([CH3:8])[O:6][CH2:5][CH:3]([O:2][CH3:1])[CH3:4])(=[O:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

6

反応物 3

HCID 243Benzoic AcidHCID 1140TolueneHCID 25485Dipropyleneglycol monomethyl ether

生成物 1

HCID 23036605Dipropylene Glycol Monomethyl Ether Benzoate収率 91.8%

試薬・触媒・溶媒 2

HCID 3084632Zirconium carbonate触媒HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

Dipropylene glycol monomethyl ether (444.6 grams; 3.0 mol), benzoic acid (373.7 grams; 3.06 mol), toluene (50 ml) and zirconium carbonate (2.0 grams) were placed into a 200 ml, 3-necked round bottom flask equipped with stirrer, thermometer, heating mantle, Dean Stark water trap, condenser and 10" Vigneux column. The reaction temperature was 180° C. at the beginning of the reaction and 217° C. after 6.5 hours with stirring. During that time, water (44 mls) was removed. The reaction was continued the next day for 2.5 hours at 224°-226° C. with the removal of water (56 mls.). The reaction mixture was washed at 95°-100° C. three times with sodium carbonate (15%) and then washed with water (400 ml). Then additional water (200 ml) was added and the product separated and dried at 125°, cooled to 100° C. and filtered. The desired product (694.6 grams) was obtained representing a yield of 91.8%. It assayed 99.5% with the following properties:

後処理

  1. customequipped with stirrer
  2. customThe reaction temperature was 180° C. at the beginning of the reaction and 217° C. after 6.5 hours
  3. customDuring that time, water (44 mls) was removed
  4. customfor 2.5 hours
  5. customat 224°-226° C.
  6. customwith the removal of water (56 mls.)
  7. washThe reaction mixture was washed at 95°-100° C. three times with sodium carbonate (15%)
  8. washwashed with water (400 ml)
  9. additionThen additional water (200 ml) was added
  10. customthe product separated
  11. customdried at 125°
  12. filtrationfiltered

出典と根拠

ORDレコード
ord-7683cff20f6a40bba5154b6656367f6b
出典データセット
uspto-grants-1990_08
特許番号
US04950702

関連ノート

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