Pyridine → 1,2-Propanediol, 3-((o-benzyloxy)phenoxy)-

HRID 327646

반응식

HRID 327646 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[OH:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16]1[O:18][CH:17]1[CH2:19][OH:20].N1C=CC=CC=1>C(O)C>[C:2]1([CH2:1][O:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[O:15][CH2:16][CH:17]([OH:18])[CH2:19][OH:20])[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 11164GlycidolHCID 804592-Benzyloxyphenol

생성물 1

HCID 30220521,2-Propanediol, 3-((o-benzyloxy)phenoxy)-수율 73%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 49.6 g (0.248 mole) of 2-benzyloxyphenol, 22.2 g (0.3 mole) of glycidol, 2 ml of pyridine and 150 ml of absolute ethanol was heated at reflux overnight. The dark solution was concentrated to give an oil which gradually crystallized. The solid was purified by column chromatography on 1.2 kg of silica gel eluted with 0-25% acetone in benzene. Appropriate fractions were combined and concentrated to yield 49.5 g (73%) of the title compound as a white solid, mp 84°-85° C. (carbon tetrachloride) (lit.1 mp 81°-82.5° C.).

후처리

  1. temperatureat reflux overnight
  2. concentrationThe dark solution was concentrated
  3. customto give an oil which
  4. customgradually crystallized
  5. customThe solid was purified by column chromatography on 1.2 kg of silica gel
  6. washeluted with 0-25% acetone in benzene
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c8b2f1c968664e6e8f59e35c9755838e
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05273993

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