Diphosgene → HCID 10998791、化合物

HRID 846291ノート

反応式

HRID 846291 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[S:4][C:5]([C:9](O)=[O:10])=[C:6]([CH3:8])[N:7]=1.[Cl:14]C(OC(Cl)(Cl)Cl)=O>ClC1C=CC=CC=1.N1C=CC=CC=1>[F:1][C:2]([F:13])([F:12])[C:3]1[S:4][C:5]([C:9]([Cl:14])=[O:10])=[C:6]([CH3:8])[N:7]=1

参加物

5

反応物 2

HCID 10426DiphosgeneHCID 108999004-Methyl-2-(trifluoromethyl)-1,3-thiazole-5-carboxylic acid

生成物 1

HCID 10998791HCID 10998791、化合物収率 98%

試薬・触媒・溶媒 2

HCID 1049Pyridine触媒HCID 7964Chlorobenzene溶媒

実験手順

In a similar apparatus to Example 1, 4.2 g (0.02 mole) of 2-trifluoromethyl-4-methylthiazole-5-carboxylic acid were suspended in 100 ml of chlorobenzene, followed by the addition of 0.04 g of pyridine. Under heating and reflux, 9.9 g (0.05 mole) of trichloromethyl chloroformate were added dropwise over 5 hours. After completion of the dropwise addition, stirring was continued for additional 2 hours. After completion of the reaction, the reaction mixture was filtered and the filtrate was concentrated to obtain 4.5 g of 2-trifluoromethyl-4-methylthiazole-5-carboxylic acid chloride. Its purity and yield were 98.7% and 98.0%, respectively.

後処理

  1. temperatureUnder heating
  2. temperaturereflux
  3. additionAfter completion of the dropwise addition
  4. customAfter completion of the reaction
  5. filtrationthe reaction mixture was filtered
  6. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-2bdc6714dcb7439ba6c6637e0ccccbfb
出典データセット
uspto-grants-1992_08
特許番号
US05136042

反応ノート

読み込み中…