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Hydrochloric Acid → 4-Amino-6-methyl-2,5-dihydro-1,2,4-triazin-3-one

HRID 265615
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HRID 265615 반응식
C([NH:4][N:5]1[CH2:10][C:9]([CH3:11])=[N:8][NH:7][C:6]1=[O:12])(=O)C.Cl.C([O-])(=O)C.[Na+]>CO>[NH2:4][N:5]1[CH2:10][C:9]([CH3:11])=[N:8][NH:7][C:6]1=[O:12]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 517045Sodium AcetateHCID 11008343N-(6-Methyl-3-oxo-2,5-dihydro-1,2,4-triazin-4(3H)-yl)acetamide

생성물 1

HCID 109755004-Amino-6-methyl-2,5-dihydro-1,2,4-triazin-3-one

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

A mixture of 85 g of 4-acetylamino-6-methyl-3-oxo-2,3,4,5-tetrahydro- 1,2,4-triazine, 63 ml of hydrochloric acid (37%) and 250 ml of methanol is stirred for 4 hours at 50° C. After cooling to 15° C., 82 g of sodium acetate are added, the mixture is stirred for a further 15 minutes, and the solvent is removed by evaporation. The residue is taken up in 100 ml of ethanol, and the solvent is removed again in vacuo. The residue is taken up in 1200 ml of acetonitrile, undissolved salt precipitates are filtered off, the filtrate is evaporated to dryness, the residue is caused to crystallize by adding 50 ml of acetic acid ethyl ester at ambient temperature, and the crystals are filtered off and dried yielding 54.6 g (85% of the theoretical amount) of the title compound having a melting point of 113°-118° C.

후처리

  1. temperatureAfter cooling to 15° C.
  2. stirringthe mixture is stirred for a further 15 minutes
  3. customthe solvent is removed by evaporation
  4. customthe solvent is removed again in vacuo
  5. customundissolved salt precipitates
  6. filtrationare filtered off
  7. customthe filtrate is evaporated to dryness
  8. customto crystallize
  9. additionby adding 50 ml of acetic acid ethyl ester at ambient temperature
  10. filtrationthe crystals are filtered off
  11. customdried

출처 및 근거

ORD 기록
ord-ad18e7bb6ec042939d38f014dd918ce5
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05648487

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