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

HRID 1067922
ノート
印刷プレビュー

反応式

HRID 1067922 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6329MethylamineHCID 22617107HCID 22617107、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-81b1faec81694c1a8421978126d0bfff
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06248900B1

反応ノート

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