Hydrochloric Acid → 3-(2-Ethyl-4-tetradecylphenoxy)-1,2-propanediol

HRID 329979노트

반응식

HRID 329979 반응식
[CH2:1]([C:3]1[CH:17]=[C:16]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[CH:15]=[CH:14][C:4]=1[O:5][CH2:6][CH:7]1[CH2:11][O:10]C(C)(C)[O:8]1)[CH3:2].Cl>O1CCCC1>[CH2:1]([C:3]1[CH:17]=[C:16]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[CH:15]=[CH:14][C:4]=1[O:5][CH2:6][CH:7]([OH:8])[CH2:11][OH:10])[CH3:2]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 142562074-((2-Ethyl-4-tetradecylphenoxy)methyl)-2,2-dimethyl-1,3-dioxolane

생성물 1

HCID 142561973-(2-Ethyl-4-tetradecylphenoxy)-1,2-propanediol수율 85.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 15.55 g of 4-[(2-ethyl-4-tetradecylphenoxy)methyl]-2,2-dimethyl-1,3-dioxolane, 10 ml of 5% hydrochloric acid and 300 ml of tetrahydrofuran was heated at reflux for 4 hours, then cooled and 1/2 of the solvent evaporated at reduced pressure. The remainder was diluted with ethyl acetate, washed with aqueous sodium bicarbonate, dried and the solvents evaporated. The residue was chromatographed on silica gel, eluting first with hexane:ethyl acetate (8:1), then (4:1), giving 12.1 g of the desired compound, mp 55°-56° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 4 hours
  3. temperaturecooled
  4. custom1/2 of the solvent evaporated at reduced pressure
  5. additionThe remainder was diluted with ethyl acetate
  6. washwashed with aqueous sodium bicarbonate
  7. customdried
  8. customthe solvents evaporated
  9. customThe residue was chromatographed on silica gel
  10. washeluting first with hexane:ethyl acetate (8:1)

출처 및 근거

ORD 기록
ord-095330ebf5c34337b7d708ec452fb188
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04894367

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