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Methylamine → 2,4-Dihydro-4-methyl-5-propoxy-3H-1,2,4-triazol-3-one

HRID 1067922
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HRID 1067922 반응식
[CH2:1]([O:4][C:5](OCCC)=[N:6][NH:7][C:8]([O:10]C)=O)[CH2:2][CH3:3].[CH3:16][NH2:17]>CO.C(O)C>[CH2:1]([O:4][C:5]1[N:17]([CH3:16])[C:8](=[O:10])[NH:7][N:6]=1)[CH2:2][CH3:3]
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참가 물질

5

반응물 2

HCID 6329MethylamineHCID 22617107HCID 22617107, 화합물

생성물 1

HCID 113210922,4-Dihydro-4-methyl-5-propoxy-3H-1,2,4-triazol-3-one

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

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온도
100 °C

실험 절차

693.6 g (94.4%) of methyl N′-dipropoxymethylenehydrazinecarboxylate (3 mol) were dissolved in 1752 g of methanol and admixed with 564.7 g (6 mol) of methylamine, dissolved in ethanol, and the mixture was heated in an autoclave at 100° C. for 20 hours. The reaction mixture was concentrated under reduced pressure, the residue was taken up in water (880 ml) the mixture was extracted with methylene chloride and the extract was concentrated under reduced pressure. The crystals which precipitated out on cooling were filtered off and dried. This gave 383 g (71.2%, content 87.6%) of 5-propoxy-4-methyl-2,4-dihydro-1,2,4-triazol-3-one in the form of a solid. Melting point: 72.5-73.5° C.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. extractionwas extracted with methylene chloride
  3. concentrationthe extract was concentrated under reduced pressure
  4. customThe crystals which precipitated out
  5. temperatureon cooling
  6. filtrationwere filtered off
  7. customdried

출처 및 근거

ORD 기록
ord-81b1faec81694c1a8421978126d0bfff
출처 데이터셋
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06248900B1

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