Hydrochloric Acid → HCID 20535105, 화합물

HRID 1680936노트

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HRID 1680936 반응식
[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]

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 96623Methoxyacetyl chlorideHCID 20535125HCID 20535125, 화합물

생성물 1

HCID 20535105HCID 20535105, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매2회HCID 8471Triethylamine용매

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온도
5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-504e016bb80347938b8c00fc743cfeda
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04276417

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