Epichlorohydrin → HCID 13157038, 화합물

HRID 964010노트

반응식

HRID 964010 반응식
[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

참가 물질

5

반응물 3

HCID 7835EpichlorohydrinHCID 113181,2-DihydroxynaphthaleneHCID 14797Potassium Hydroxide

생성물 1

HCID 13157038HCID 13157038, 화합물수율 74.1%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bf249c08c4b249578a1c3b95f839accf
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05767116

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