Ethanolamine → 3-(5-NITRO-1-METHYL-2-IMIDAZOLYL)-6-(beta-HYDROXYETHYL-AMINOMETHYLENEAMINO)-S-TRIAZOLO[4,3-b]PYRIDAZINE

HRID 1729873노트

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HRID 1729873 반응식
[N+](C1N(C)C(C2N3N=C(N=C[O:21][CH2:22][CH3:23])C=CC3=NN=2)=NC=1)([O-])=O.C(CN)O.[N+:28]([C:31]1[N:35]([CH3:36])[C:34]([C:37]2[N:41]3[N:42]=[C:43]([N:46]=[CH:47][NH:48]CCO)[CH:44]=[CH:45][C:40]3=[N:39][N:38]=2)=[N:33][CH:32]=1)([O-:30])=[O:29]>C(O)(C)C.O1CCOCC1>[N+:28]([C:31]1[N:35]([CH3:36])[C:34]([C:37]2[N:41]3[N:42]=[C:43]([N:46]=[C:47]([CH2:23][CH2:22][OH:21])[NH2:48])[CH:44]=[CH:45][C:40]3=[N:39][N:38]=2)=[N:33][CH:32]=1)([O-:30])=[O:29]

참가 물질

5

반응물 3

HCID 700EthanolamineHCID 214559113-(5-Nitro-1-methyl-2-imidazolyl)-6-ethoxymethyleneamino-s-triazolo[4,3-b]pyridazineHCID 178481317HCID 178481317, 화합물

생성물 1

HCID 867341263-(5-NITRO-1-METHYL-2-IMIDAZOLYL)-6-(beta-HYDROXYETHYL-AMINOMETHYLENEAMINO)-S-TRIAZOLO[4,3-b]PYRIDAZINE

시약·촉매·용매 1

HCID 20284604Dioxane isopropanol용매

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온도
20 °C

실험 절차

1.2 g. crude 3-(5-nitro-1-methyl-2-imidazolyl)-6-ethoxymethyleneamino-s-triazolo[4,3-b]pyridazine was dissolved in 13 ml. isopropanol-dioxan mixture (7:3), 1 ml. ethanolamine was added thereto at 20° C., while stirring, and stirring was then continued for 30 minutes. The precipitated crystals were filtered off with suction, washed with isopropanol and water and dried for 2 hours at 120° C. in a vacuum. There was obtained 1.07 g. of the desired 3-(5-nitro-1-methyl-2-imidazolyl)-6-(β-hydroxyethylaminomethyleneamino)-s-triazolo[4,3-b]pyridazine, which has a melting point of 191° - 192° C.

후처리

  1. stirringstirring
  2. filtrationThe precipitated crystals were filtered off with suction
  3. washwashed with isopropanol and water
  4. customdried for 2 hours at 120° C. in a vacuum
  5. customThere was obtained 1.07 g

출처 및 근거

ORD 기록
ord-5361e57088304b2eb79a275b37e774c1
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03989832

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