Diethyl Ether → HCID 19978122, 화합물

HRID 1449511노트

반응식

HRID 1449511 반응식
[ClH:1].[CH2:2]([C:5]1[N:9]2[CH2:10][CH2:11][CH2:12][N:13]=[C:8]2[S:7][C:6]=1[C:14]([OH:16])=O)[CH2:3][CH3:4].C(OCC)C>S(Cl)(Cl)=O>[ClH:1].[CH2:2]([C:5]1[N:9]2[CH2:10][CH2:11][CH2:12][N:13]=[C:8]2[S:7][C:6]=1[C:14]([Cl:1])=[O:16])[CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 3283Diethyl EtherHCID 67715287HCID 67715287, 화합물

생성물 1

HCID 19978122HCID 19978122, 화합물수율 203.8%

시약·촉매·용매 1

HCID 24386Thionyl Chloride용매

실험 절차

In 35 ml of thionyl chloride was suspended 5.3 g of 3-propyl-6,7-dihydro-5H-thiazolo[3,2-a]pyrimidine-2-carboxylic acid hydrochloride obtained Example 12, followed by reflux under heating for 40 minutes. The reaction mixture was cooled with ice, and poured into dry diethyl ether. The precipitated crystals were collected by filtration to yield 5.78 g of 3-propyl-6,7-dihydro-5H-thiazolo[3,2-a]pyrimidine-2-carbonyl chloride hydrochloride as colorless powder. This powder was suspended in the mixture of 200 ml of pyridine and 20 ml of dimethylformamide. To the mixture were added 3.38 g of 3.5-dichloroaniline and 250 mg of 3,5-dimethyl-aminopyridine, followed by stirring at 60° C. for 18 hours. The reaction mixture was concentrated and to the mixture was added water. The precipitated crystals were collected by filtration, washed successively with water and cold methanol and suspended in ethanol. To the mixture was added saturated hydrogenchloride diethylether. The formed crystals were collected by filtration and recrystallized from ethanol to obtain 3.65 g of the titled compound.

후처리

  1. customobtained Example 12
  2. temperatureby reflux
  3. temperatureunder heating for 40 minutes
  4. temperatureThe reaction mixture was cooled with ice
  5. filtrationThe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-f98efdc28ef64b518f99773444238554
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599813

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