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Methyl chloroformate → HCID 21561613, 화합물

HRID 1581132
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HRID 1581132 반응식
Cl.[OH:2][CH2:3][C:4]1[CH:5]=[C:6]([OH:11])[C:7]([CH3:10])=[N:8][CH:9]=1.[C:12](Cl)(=[O:15])[O:13][CH3:14]>N1C=CC=CC=1>[CH3:14][O:13][C:12]([O:2][CH2:3][C:4]1[CH:5]=[C:6]([OH:11])[C:7]([CH3:10])=[N:8][CH:9]=1)=[O:15]
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참가 물질

4

반응물 2

HCID 6586Methyl chloroformateHCID 1991873-Pyridinemethanol, 5-hydroxy-6-methyl-, hydrochloride

생성물 1

HCID 21561613HCID 21561613, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of 1.8 g. of 5-hydroxymethyl-2-methyl-3-pyridinol hydrochloride in 10 ml. of pyridine was added 1.0 g. of methyl chlorocarbonate dropwise under cooling. After standing overnight, the reaction mixture was poured into ice water and extracted with ethyl acetate. The extract was washed with water, dried and the solvent was distilled off to give 1.0 g. of an oily substance. The oily substance was purified by column chromatography (silica gel 20 g.) and 0.6 g. of the desired product as colorless crystal was obtained from the eluate with benzene-ethyl acetate (3:7) and recrystallized from ethyl acetate and n-hexane.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. distillationthe solvent was distilled off
  5. customto give 1.0 g
  6. customThe oily substance was purified by column chromatography (silica gel 20 g.) and 0.6 g

출처 및 근거

ORD 기록
ord-85d180ccb81f4501a7d653f6e4941035
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03935311

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