Hydrochloric Acid → 3-(2-Ethyl-5-tetradecylphenoxy)1,2-propanediol

HRID 703340노트

반응식

HRID 703340 반응식
[CH2:1]([C:3]1[CH:17]=[CH:16][C:15]([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: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]=[CH:16][C:15]([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: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 148196794-((2-Ethyl-5-tetradecylphenoxy)methyl)-2,2-dimethyl-1,3-dioxolane

생성물 1

HCID 142562013-(2-Ethyl-5-tetradecylphenoxy)1,2-propanediol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 14.2 g of 4-[(2-ethyl-5-tetradecylphenoxy)methyl]-2,2-dimethyl-1,3-dioxolane, 50 ml of 5% hydrochloric acid and 100 ml of tetrahydrofuran was heated at reflux for 8 hours, then allowed to cool and the tetrahydrofuran removed under reduced pressure. Ethyl acetate was added, the mixture washed with water, dried and the solvents removed. The residue was chromatographed on silica gel, eluting impurites with hexane:ethyl acetate (16:1) and then (4:1) to elute the desired compound, giving 11 g, 55.5°-56.5° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 8 hours
  3. temperatureto cool
  4. customthe tetrahydrofuran removed under reduced pressure
  5. additionEthyl acetate was added
  6. washthe mixture washed with water
  7. customdried
  8. customthe solvents removed
  9. customThe residue was chromatographed on silica gel
  10. washeluting impurites with hexane:ethyl acetate (16:1)
  11. wash(4:1) to elute the desired compound
  12. customgiving 11 g, 55.5°-56.5° C.

출처 및 근거

ORD 기록
ord-970b02c955974e2d957764549ce1b2e4
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04981989

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