Hydrochloric Acid → HCID 20535123, 화합물

HRID 1680927노트

반응식

HRID 1680927 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.[C:19]1([CH2:25][C:26](Cl)=[O:27])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.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:26](=[O:27])[CH2:25][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[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 7679Phenylacetyl chlorideHCID 20535125HCID 20535125, 화합물

생성물 1

HCID 20535123HCID 20535123, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매2회HCID 8471Triethylamine용매

실험 절차

4.5 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. 4.8 ml. of phenylacetyl chloride in 30 ml. of methylene chloride are added dropwise while stirring and cooling. The mixture is then stirred at room temperature for 70 minutes, 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 to dryness 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-phenyl-acetamide having a melting point of 165°-167° C.

후처리

  1. temperaturecooling
  2. stirringThe mixture is then stirred at room temperature for 70 minutes
  3. customThe two phases are separated
  4. extractionthe aqueous phase is extracted with methylene chloride
  5. dry with materialThe combined organic extracts are dried over sodium sulfate
  6. customevaporated to dryness under reduced pressure
  7. customThe residue is recrystallized from methylene chloride and diethyl ether, there

출처 및 근거

ORD 기록
ord-38d32039d1e5488890faa40d7a845080
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04276417

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