Diphosgene → 4-Chloro-2,3-dihydro-2,2-dimethylbenzofuran-7-yl isocyanate

HRID 440654ノート

反応式

HRID 440654 の反応式
[NH2:1][C:2]1[C:10]2[O:9][C:8]([CH3:12])([CH3:11])[CH2:7][C:6]=2[C:5]([Cl:13])=[CH:4][CH:3]=1.Cl[C:15](OC(Cl)(Cl)Cl)=[O:16]>C1(C)C=CC=CC=1>[Cl:13][C:5]1[C:6]2[CH2:7][C:8]([CH3:11])([CH3:12])[O:9][C:10]=2[C:2]([N:1]=[C:15]=[O:16])=[CH:3][CH:4]=1

参加物

4

反応物 2

HCID 10426DiphosgeneHCID 224047737-Amino-4-chloro-2,3-dihydro-2,2-dimethylbenzofuran

生成物 1

HCID 153462864-Chloro-2,3-dihydro-2,2-dimethylbenzofuran-7-yl isocyanate収率 99.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of 1.97 g (0.010 mole) of 7-amino-4-chloro-2,3-dihydro-2,2-dimethylbenzofuran in 60 mL of toluene was added slowly 1.2 mL (0.010 mole) of trichloromethyl chloroformate. This mixture was stirred at ambient temperature for one hour and then was heated at reflux for approximately 16 hours. At the conclusion of this period the solvent was evaporated from the reaction mixture under reduced pressure, leaving 2.23 g of 4-chloro-2,3-dihydro-2,2-dimethylbenzofuran-7-yl isocyanate as an oil.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for approximately 16 hours
  3. customAt the conclusion of this period the solvent was evaporated from the reaction mixture under reduced pressure

出典と根拠

ORDレコード
ord-89ed21e2b5e043df8fc9252b13124aa5
出典データセット
uspto-grants-1996_05
特許番号
US05521147

反応ノート

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