Phosgene → 2-Ethyl-4-methyl-1,3-thiazole-5-carbonyl chloride

HRID 846296노트

반응식

HRID 846296 반응식
[CH2:1]([C:3]1[S:4][C:5]([C:9]([OH:11])=O)=[C:6]([CH3:8])[N:7]=1)[CH3:2].CN(C)C(=O)C.C(Cl)([Cl:20])=O>C1(C)C=CC=CC=1>[CH2:1]([C:3]1[S:4][C:5]([C:9]([Cl:20])=[O:11])=[C:6]([CH3:8])[N:7]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 6371PhosgeneHCID 31374DimethylacetamideHCID 138352922-Ethyl-4-methyl-1,3-thiazole-5-carboxylic acid

생성물 1

HCID 147162072-Ethyl-4-methyl-1,3-thiazole-5-carbonyl chloride

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

In a similar apparatus to Example 1, 15.0 g (0.09 mole) of 2-ethyl-4-methylthiazole-5-carboxylic acid were suspended in 150 ml of toluene, followed by the addition of 0.1 g of N,N-dimethylacetamide. Under heating and reflux, phosgene was blown at a rate of 1.5 l/hr for 3.5 hours (0.23 mole). After completion of the reaction, the reaction mixture was filtered and the filtrate was concentrated to obtain 16.1 g of 2-ethyl-4-methylthiazole-5-carboxylic acid chloride. Its purity and yield were 98.2% and 96.9%, respectively.

후처리

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

출처 및 근거

ORD 기록
ord-dbf1dd08c8d1453fb60aa7594a78fb57
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05136042

반응 노트

불러오는 중…