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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Methyl chloroformate → HCID 21561613、化合物

HRID 1581132
ノート
印刷プレビュー

反応式

HRID 1581132 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 21561613HCID 21561613、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-85d180ccb81f4501a7d653f6e4941035
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03935311

反応ノート

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