Pyridine → HCID 54501726、化合物

HRID 1449523ノート

反応式

HRID 1449523 の反応式
[N:1]1[CH:6]=CC=C[CH:2]=1.Cl.C([C:11]1[N:15]2[CH2:16][CH2:17][CH2:18][N:19]=[C:14]2SC=1C(Cl)=O)CC.C(SC1C=CC(N)=CC=1)CCCCCC>CN(C)C=O>[CH3:11][NH:15][C:16]1[CH:2]=[N:1][CH:6]=[C:18]([NH:19][CH3:14])[CH:17]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 14044811HCID 14044811、化合物HCID 19978122HCID 19978122、化合物

生成物 1

HCID 54501726HCID 54501726、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In the mixture of 50 ml of pyridine and 5 ml of dimethylformamide was suspended 1.07 g of 3-propyl-6,7-dihydro-5H-thiazolo[3,2-a]pyrimidine-2-carbonylchloride hydrochloride (described in Example 13). To the suspension were added 850 mg of 4-n-heptylthioaniline obtained in Reference Example 6, and 56 mg of 3,5-dimethylaminopyridine, followed by stirring at 70° C. for 12 hours. The reaction mixture was concentrated and to the concentrate was added saturated sodium hydrogencarbonate aqueous solution. The mixture was extracted with chloroform. The extract was washed with saturated sodium chloride aqueous solution, dried over anhydrous potassium carbonate and treated with active carbon. The solvent was removed under reduced pressure. The residue was dissolved in ethanol. To the mixture was added saturated hydrogenchloride diethylether solution, followed by stirring at room temperature. The solvent was removed under reduced pressure. The residue was precipitated from ethanol-diethylether to collect by filtration. The precipitated powder was recrystallized from methanoldiethylether to yield 992 mg of the titled compound.

出典と根拠

ORDレコード
ord-702f7ef0cf51474b951af0e9aa563034
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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