Guaiacol → 2-Methoxyphenyl chloroformate

HRID 896450

反応式

HRID 896450 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1O.CN(C)C1C=CC=CC=1.[C:19]([Cl:22])(Cl)=[O:20].CN(C=[O:27])C>C1(C)C=CC=CC=1.ClC1C=CC=CC=1>[Cl:22][C:19]([O:20][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[O:2][CH3:1])=[O:27]

参加物

7

反応物 4

HCID 460GuaiacolHCID 949N,N-DimethylanilineHCID 6228DimethylformamideHCID 6371Phosgene

生成物 1

HCID 33621432-Methoxyphenyl chloroformate収率 50%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 7964Chlorobenzene溶媒

実験手順

A solution of 2-methoxyphenol (2 g, 16.1 mmol), N,N-dimethylaniline (1.95 g, 16.1 mmol), phosgene (8.34 mL of a 1.93 M solution in toluene, 16.1 mmol) and a catalytic amount of DMF in chlorobenzene (5 mL) was stirred in a pressure tube for 2 h at 80° C. The organic layer was separated and concentrated in vacuo. The residue was distilled (Buchi Kugelrohr; bp=115° C. @ 10 mm Hg) to provide 2-methoxyphenyl chloroformate (1.5 g; 50%) as a clear oil.

後処理

  1. customThe organic layer was separated
  2. concentrationconcentrated in vacuo
  3. distillationThe residue was distilled (Buchi Kugelrohr; bp=115° C. @ 10 mm Hg)

出典と根拠

ORDレコード
ord-6883fa29facc45709c9dfab329d65053
出典データセット
uspto-grants-2005_07
特許番号
US06919358B2

関連ノート

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