Epichlorohydrin → HCID 13157038、化合物

HRID 964010ノート

反応式

HRID 964010 の反応式
[CH2:1]([CH:3]1[O:5][CH2:4]1)Cl.[OH:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:10]=[CH:9][C:8]=1[OH:17].[OH-].[K+]>O>[O:6]1[CH:3]([CH2:4][OH:5])[CH2:1][O:17][C:8]2[CH:9]=[CH:10][C:11]3[C:16]([C:7]1=2)=[CH:15][CH:14]=[CH:13][CH:12]=3

参加物

5

反応物 3

HCID 7835EpichlorohydrinHCID 113181,2-DihydroxynaphthaleneHCID 14797Potassium Hydroxide

生成物 1

HCID 13157038HCID 13157038、化合物収率 74.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Epichlorohydrin (2.32 g) was added dropwise to a stirred solution of 1,2-dihydroxynaphthalene (4.0 g) and potassium hydroxide (4.0 g) in water (32 ml) and the resulting mixture stirred at 60°-80° C. for 2.5 hours then poured into water (100 ml). The product was extracted into ether (6×100 ml), a small volume of methanol being added to aid solubility. The combined extracts were washed with aqueous sodium hydroxide solution (1M), then water, and dried over magnesium sulphate. The solvent was removed in vacuo to give crude 1-(naphtho[1,2-b]dioxan-2-yl)methanol (4.0 g) as a dark oil which was used without further purification.

後処理

  1. extractionThe product was extracted into ether (6×100 ml)
  2. additiona small volume of methanol being added
  3. washThe combined extracts were washed with aqueous sodium hydroxide solution (1M)
  4. dry with materialwater, and dried over magnesium sulphate
  5. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-bf249c08c4b249578a1c3b95f839accf
出典データセット
uspto-grants-1998_06
特許番号
US05767116

反応ノート

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