Hydrochloric Acid → HCID 20535105、化合物

HRID 1680936ノート

反応式

HRID 1680936 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.[CH3:19][O:20][CH2:21][C:22](Cl)=[O:23].Cl>O.C(Cl)Cl.C(N(CC)CC)C>[CH2:13]([N:12]([CH2:16][CH:17]=[CH2:18])[C:4]1[N:3]=[C:2]([NH:1][C:22](=[O:23])[CH2:21][O:20][CH3:19])[N:7]2[O:8][C:9](=[O:11])[N:10]=[C:6]2[N:5]=1)[CH:14]=[CH2:15]

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 96623Methoxyacetyl chlorideHCID 20535125HCID 20535125、化合物

生成物 1

HCID 20535105HCID 20535105、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回HCID 8471Triethylamine溶媒

反応条件

温度
5 °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 100 ml. of methylene chloride and 10 ml. of triethylamine. 2.5 g. of methoxyacetyl chloride in 20 ml. of methylene chloride are added dropwise while stirring and cooling to about 5° C. After 1 hour at about 5° C., the mixture is treated with water and adjusted to pH 4 with 3-N hydrochloric acid. The two phases are separated and the aqueous phase is extracted with methylene chloride. The combined organic extracts are dried over sodium sulfate and evaporated under reduced pressure. The residue is recrystallized from methylene chloride and diethyl ether, there being obtained N-{5-diallylamino-2-oxo-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazin-7-yl}-2-methoxyacetamide having a melting point of 135°-136° C.

後処理

  1. customThe two phases are separated
  2. extractionthe aqueous phase is extracted with methylene chloride
  3. dry with materialThe combined organic extracts are dried over sodium sulfate
  4. customevaporated under reduced pressure
  5. customThe residue is recrystallized from methylene chloride and diethyl ether, there

出典と根拠

ORDレコード
ord-504e016bb80347938b8c00fc743cfeda
出典データセット
uspto-grants-1981_06
特許番号
US04276417

反応ノート

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