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

HRID 703340ノート

反応式

HRID 703340 の反応式
[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]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 148196794-((2-Ethyl-5-tetradecylphenoxy)methyl)-2,2-dimethyl-1,3-dioxolane

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-970b02c955974e2d957764549ce1b2e4
出典データセット
uspto-grants-1991_01
特許番号
US04981989

反応ノート

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