Diethyl Ether → HCID 19978122、化合物

HRID 1449511ノート

反応式

HRID 1449511 の反応式
[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]

参加物

4

反応物 2

HCID 3283Diethyl EtherHCID 67715287HCID 67715287、化合物

生成物 1

HCID 19978122HCID 19978122、化合物収率 203.8%

試薬・触媒・溶媒 1

HCID 24386Thionyl Chloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f98efdc28ef64b518f99773444238554
出典データセット
uspto-grants-1997_02
特許番号
US05599813

反応ノート

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