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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
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반응식

HRID 26495 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5cebb67da49945f99aaa3c98a0cda91a
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04150139

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