Oxalyl chloride → Benzoyl isocyanate, 2-chloro-4-fluoro-

HRID 887895ノート

反応式

HRID 887895 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].C(Cl)(=O)[C:13](Cl)=[O:14]>ClCCl>[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([N:6]=[C:13]=[O:14])=[O:5]

参加物

4

反応物 2

HCID 65578Oxalyl chlorideHCID 5228982-Chloro-4-fluorobenzamide

生成物 1

HCID 11521269Benzoyl isocyanate, 2-chloro-4-fluoro-収率 96.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1.64 g (6 mmol) of 2-chloro-4-fluorobenzamide were dissolved in 3 ml of dichloromethane and, at 0° C. and under a nitrogen atmosphere, 0.8 ml (9.3 mmol) of oxalyl chloride was added, and the mixture was heated to reflux for 9 hours. The reaction mixture was concentrated under high vacuum and afforded 1.17 g (5.8 mmol) of the desired product, which was employed as solution in dichloromethane (1 mmol in 1.7 ml of solution) in stage b.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 9 hours
  3. concentrationThe reaction mixture was concentrated under high vacuum

出典と根拠

ORDレコード
ord-a6e6fdec1ffb4fef80867eba3eabc620
出典データセット
uspto-grants-2012_08
特許番号
US08247452B2

反応ノート

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