Diphosgene → HCID 10998791, 화합물

HRID 846291노트

반응식

HRID 846291 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 10998791HCID 10998791, 화합물수율 98%

시약·촉매·용매 2

HCID 1049Pyridine촉매HCID 7964Chlorobenzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2bdc6714dcb7439ba6c6637e0ccccbfb
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05136042

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