Pyridine → 3-Pyridinyl carbonochloridate

HRID 2297642ノート

反応式

HRID 2297642 の反応式
[C:1](Cl)([Cl:3])=[O:2].C1(C)C=CC=CC=1.[OH:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1.N1C=CC=CC=1>C(Cl)Cl>[Cl:3][C:1]([O:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1)=[O:2]

参加物

6

反応物 4

HCID 1049PyridineHCID 1140TolueneHCID 6371PhosgeneHCID 79713-Hydroxypyridine

生成物 1

HCID 154347383-Pyridinyl carbonochloridate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A 1.93M solution of phosgene in toluene (20%) (198.3 ml) (382.3 mmoles) was diluted with dry CH2Cl2 (100 ml) and the mixture was stirred at 0° under an argon atmosphere. A solution of 3-hydroxy-pyridine (7.27 grams) (76.5 mmoles) and dry pyridine (8.06 grams) (8.25 ml) (101.9 mmoles) in dry CH2Cl2 (200 ml) was added dropwise to the stirred solution at 0° over a period of 1 hour. The mixture was stirred at 0-25° for an additional 2 hours. A stream of nitrogen was passed through the solution to remove most of the phosgene and the solution was then evaporated to dryness to give the title compound which was dried in vacuo for 1 hour and then taken up in dry CH2Cl2 (60 ml) and dry pyridine (60 ml) to give a stock solution of the title compound.

後処理

  1. stirringThe mixture was stirred at 0-25° for an additional 2 hours
  2. customto remove most of the phosgene
  3. customthe solution was then evaporated to dryness

出典と根拠

ORDレコード
ord-16ad87e5f3bd4b548eb243d2cd12e7c9
出典データセット
uspto-grants-2002_12
特許番号
US06492381B1

反応ノート

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