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Hydrochloric Acid → 1-(3-benzyl-1,5-dihydro-5-thioxo-4H-1,2,4-triazol-4-yl)-2-propanone

HRID 26495
ノート
印刷プレビュー

反応式

HRID 26495 の反応式
C1O[C:4]([CH3:19])([CH2:5][N:6]2[C:10](=[S:11])[NH:9][N:8]=[C:7]2[CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[O:3]C1.Cl>C(O)C>[CH2:12]([C:7]1[N:6]([CH2:5][C:4](=[O:3])[CH3:19])[C:10](=[S:11])[NH:9][N:8]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 213235511-(3-benzyl-1,5-dihydro-5-thioxo-4H-1,2,4-triazol-4-yl)-2-propanone ethylenacetal

生成物 1

HCID 213234591-(3-benzyl-1,5-dihydro-5-thioxo-4H-1,2,4-triazol-4-yl)-2-propanone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 10 ml of ethanol was added 1.1 g of the 1-(3-benzyl-1,5-dihydro-5-thioxo-4H-1,2,4-triazol-4-yl)-2-propanone ethylenacetal obtained in Reference Example 5, followed by addition of 5.0 ml of 2N-hydrochloric acid. The mixture was refluxed for 40 minutes and, then, concentrated to half the original volume. To the concentrate was added water and the resultant precipitate was recovered by filtration. This procedure provided 1-(3-benzyl-1,5-dihydro-5-thioxo-4H-1,2,4-triazol-4-yl)-2-propanone as crystals. Recrystallization from ethyl acetate gave colorless needles melting at 163°-165° C.

後処理

  1. customobtained in Reference Example 5
  2. temperatureThe mixture was refluxed for 40 minutes
  3. concentrationconcentrated to half the original volume
  4. additionTo the concentrate was added water
  5. filtrationthe resultant precipitate was recovered by filtration

出典と根拠

ORDレコード
ord-5cebb67da49945f99aaa3c98a0cda91a
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04150139

反応ノート

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