Hydrochloric Acid → HCID 20535132, 화합물

HRID 1680929노트

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HRID 1680929 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(Cl)(Cl)Cl.[Cl:23][C:24]1[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[C:25]=1[C:26](Cl)=[O:27].Cl>O.C(N(CC)CC)C>[Cl:23][C:24]1[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[C:25]=1[C:26]([NH: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)=[O:27]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 783922,6-Dichlorobenzoyl chlorideHCID 20535125HCID 20535125, 화합물

생성물 1

HCID 20535132HCID 20535132, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8471Triethylamine용매

실험 절차

5.0 g. of 7-amino-5-diallylamino-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazin-2-one are mixed with 150 ml. of chloroform, 10 ml. of triethylamine and 4.5 ml. of 2,6-dichlorobenzoyl chloride and heated to reflux for 7 hours. The mixture is then cooled, diluted with water, adjusted to pH 4 with hydrochloric acid and extracted with chloroform. The combined organic extracts are dried over sodium sulfate and evaporated to dryness under reduced pressure. The residue is chromatographed over silica gel using a mixture of methylene chloride and methanol (99:1) for the elution. Recrystallization from diisopropyl ether and methylene chloride yields pure 2,6-dichloro-N-{5-diallylamino-2-oxo-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazin-7-yl}benzamide having a melting point of 133°-135° C.

후처리

  1. temperatureto reflux for 7 hours
  2. temperatureThe mixture is then cooled
  3. extractionextracted with chloroform
  4. dry with materialThe combined organic extracts are dried over sodium sulfate
  5. customevaporated to dryness under reduced pressure
  6. customThe residue is chromatographed over silica gel using
  7. additiona mixture of methylene chloride and methanol (99:1)
  8. washfor the elution
  9. customRecrystallization from diisopropyl ether and methylene chloride

출처 및 근거

ORD 기록
ord-65b49f1d7b9a488b9a0237b18248f526
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04276417

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