Ammonia → 5-Thiazolecarboxamide, 2-(4-methoxyphenyl)-4-methyl-

HRID 637710

反応式

HRID 637710 の反応式
N.[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[S:11][C:12]([C:16]([O:18]CC)=O)=[C:13]([CH3:15])[N:14]=2)=[CH:6][CH:5]=1.COC1C=CC(C([NH2:29])=O)=CC=1.ClC(C(C)=O)C(OCC)=O.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=S>C(O)CCC.C(O)C>[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[S:11][C:12]([C:16]([NH2:29])=[O:18])=[C:13]([CH3:15])[N:14]=2)=[CH:6][CH:5]=1

参加物

8

反応物 5

HCID 222AmmoniaHCID 11858Ethyl 2-chloroacetoacetateHCID 14817Phosphorus sulfide (P2S5)HCID 769594-MethoxybenzamideHCID 7540952Ethyl 2-(4-methoxyphenyl)-4-methyl-1,3-thiazole-5-carboxylate

生成物 1

HCID 30680755-Thiazolecarboxamide, 2-(4-methoxyphenyl)-4-methyl-収率 69%

試薬・触媒・溶媒 2

HCID 2631-Butanol溶媒HCID 702Ethanol溶媒

実験手順

Into a mixed solvent of 50 ml of aqueous 28% ammonia and 450 ml of ethanol, 13.9 g of ethyl 2-(4-methoxyphenyl)-4-methylthiazole-5-carboxylate which had been prepared by heating a mixture of p-methoxybenzamide, ethyl α-chloroacetoacetate, phosphorus pentasulfide and n-butyl alcohol under a reflux for 5 hours was dissolved. Then, in a similar manner as in Example 3 the object was obtained as colourless aciculate melting at 179.5° to 180.5° C. in an amount of 8.6 g corresponding to the yield of 69%.

後処理

  1. temperatureby heating
  2. temperaturea reflux for 5 hours
  3. dissolutionwas dissolved
  4. customThen, in a similar manner as in Example 3 the object was obtained as colourless aciculate melting at 179.5° to 180.5° C. in an amount of 8.6 g corresponding to the yield of 69%

出典と根拠

ORDレコード
ord-09f717849cbc469691ad175eb4290b29
出典データセット
uspto-grants-1985_12
特許番号
US04558059

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