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

HRID 265614
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HRID 265614 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.O.[OH-].[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

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 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

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온도
5 °C

실험 절차

85 g of 4-acetylamino-6-methyl-3-oxo-2,3,4,5-tetrahydro-1,2,4-triazine in 250 ml of methanol are stirred together with 63 ml of hydrochloric acid (37%) for 4 hours at 50° C. After cooling to 5° C., 250 ml of icecold water and 125 ml of sodium hydroxide solution (50%) are added. The solvent is removed by evaporation in vacuo. 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 removed by filtration, the filtrate is concentrated to a small volume, the residue is caused to crystallize by adding 100 ml of acetic acid ethyl ester at 0° C., and the colorless crystals are filtered off and dried yielding 60.4 g (92% of the theoretical amount) of the title compound having a melting point of 118°-120° C.

후처리

  1. customThe solvent is removed by evaporation in vacuo
  2. customthe solvent is removed again in vacuo
  3. customundissolved salt precipitates
  4. customare removed by filtration
  5. concentrationthe filtrate is concentrated to a small volume
  6. customto crystallize
  7. additionby adding 100 ml of acetic acid ethyl ester at 0° C.
  8. filtrationthe colorless crystals are filtered off
  9. customdried

출처 및 근거

ORD 기록
ord-464ee6fdfc0d4e258978e0470fbc8dd2
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05648487

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