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

HRID 34840ノート

反応式

HRID 34840 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-55ea2f5a14db439ca59cd47390d5c2c2
出典データセット
uspto-grants-1988_08
特許番号
US04762942

反応ノート

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