Sulfuric Acid → p-n-Octadecyloxybenzoic acid

HRID 21434

반응식

HRID 21434 반응식
[CH2:1]([O:19][C:20]1[CH:29]=[CH:28][C:23]([C:24]([O:26]C)=[O:25])=[CH:22][CH:21]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].S(=O)(=O)(O)O>C(O)(=O)C>[CH2:1]([O:19][C:20]1[CH:21]=[CH:22][C:23]([C:24]([OH:26])=[O:25])=[CH:28][CH:29]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 4189536Methyl 4-(octadecyloxy)benzoate

생성물 1

HCID 139993p-n-Octadecyloxybenzoic acid수율 82.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture containing methyl 4-octadecyloxybenzoate (30 g) and acetic acid (10 ml) was warmed until a solution was obtained. To this solution was added concentrated sulfuric acid (3 ml), and the mixture heated to slowly distill off the methyl acetate. This distillation was carried out over a period of 40 minutes. The solution was then cooled just below the boiling point and stirred for an additional 30 minutes. The hot reaction mixture was poured onto cold water and the solid filtered and dried. The product was then slurried in methylene chloride (100 ml) then filtered. The solid was recrystallized from 2-butanone to give 4-octadecyloxybenzoic acid (24 g).

후처리

  1. temperaturewas warmed until a solution
  2. customwas obtained
  3. temperaturethe mixture heated
  4. distillationto slowly distill off the methyl acetate
  5. distillationThis distillation
  6. temperatureThe solution was then cooled just below the boiling point
  7. additionThe hot reaction mixture was poured onto cold water
  8. filtrationthe solid filtered
  9. customdried
  10. filtrationthen filtered
  11. customThe solid was recrystallized from 2-butanone

출처 및 근거

ORD 기록
ord-2a7c3976ac664099ac53a5193537f233
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424183

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