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

HRID 703325ノート

反応式

HRID 703325 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-8047355cf0c643cfb20ec25c14a6c95b
出典データセット
uspto-grants-1991_01
特許番号
US04981989

反応ノート

読み込み中…