Hydrochloric Acid → HCID 20535101、化合物

HRID 1156611ノート

反応式

HRID 1156611 の反応式
[NH2:1][C:2]1[N:7]2[O:8][C:9](=[O:11])[N:10]=[C:6]2[N:5]=[C:4]([N:12]([CH2:16][CH:17]=[CH2:18])[CH2:13][CH:14]=[CH2:15])[N:3]=1.C(N(CC)CC)C.[Cl:26][C:27]1[CH:35]=[CH:34][C:30]([C:31](Cl)=[O:32])=[CH:29][CH:28]=1.Cl>O.C(Cl)Cl>[Cl:26][C:27]1[CH:35]=[CH:34][C:30]([C:31]([NH:1][C:2]2[N:7]3[O:8][C:9](=[O:11])[N:10]=[C:6]3[N:5]=[C:4]([N:12]([CH2:16][CH:17]=[CH2:18])[CH2:13][CH:14]=[CH2:15])[N:3]=2)=[O:32])=[CH:29][CH:28]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 85014-Chlorobenzoyl chlorideHCID 20535125HCID 20535125、化合物

生成物 1

HCID 20535101HCID 20535101、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

5.0 g. of 7-amino-5-diallylamino-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazin-2-one are suspended in 7 ml. of triethylamine and 150 ml. of methylene chloride. 3.4 ml. of 4-chlorobenzoyl chloride in 35 ml. of methylene chloride are added dropwise while stirring and cooling to about 0° C. The mixture is subsequently stirred at about 0° C. for 1 hour. Water is then added thereto and the pH is adjusted to 4 with dilute hydrochloric acid solution. The two phases are separated and the aqueous phase is extracted twice with methylene chloride. The combined organic extracts are dried over sodium sulfate and evaporated to dryness under reduced pressure. The residue is recrystallized from methylene chloride and diethyl ether, there being obtained pure p-chloro-N-{5-diallylamino-2-oxo-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazin-7-yl}benzamide having a melting point of 192°-194° C.

後処理

  1. stirringThe mixture is subsequently stirred at about 0° C. for 1 hour
  2. customThe two phases are separated
  3. extractionthe aqueous phase is extracted twice with methylene chloride
  4. dry with materialThe combined organic extracts are dried over sodium sulfate
  5. customevaporated to dryness under reduced pressure
  6. customThe residue is recrystallized from methylene chloride and diethyl ether, there

出典と根拠

ORDレコード
ord-645860eca69c44189d4d77f9644dc87f
出典データセット
uspto-grants-1982_06
特許番号
US04336380

反応ノート

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