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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2,5-Hexanedione → alpha-[2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]-N-(2,5-dimethyl-1-pyrrolyl)acetamide

HRID 1198911
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인쇄 미리보기

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HRID 1198911 반응식
[CH2:1]([CH2:5][C:6](=O)[CH3:7])[C:2]([CH3:4])=O.[Cl:9][C:10]1[CH:21]=[C:20]([C:22]2[CH:23]([CH3:29])[NH:24][C:25](=[O:28])[NH:26][N:27]=2)[CH:19]=[CH:18][C:11]=1[O:12][CH2:13][C:14]([NH:16][NH2:17])=[O:15]>C(O)(=O)C>[Cl:9][C:10]1[CH:21]=[C:20]([C:22]2[CH:23]([CH3:29])[NH:24][C:25](=[O:28])[NH:26][N:27]=2)[CH:19]=[CH:18][C:11]=1[O:12][CH2:13][C:14]([NH:16][N:17]1[C:6]([CH3:7])=[CH:5][CH:1]=[C:2]1[CH3:4])=[O:15]
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참가 물질

4

반응물 2

HCID 80352,5-HexanedioneHCID 14370703alpha-[2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetohydrazide

생성물 1

HCID 14370704alpha-[2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]-N-(2,5-dimethyl-1-pyrrolyl)acetamide수율 64%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

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온도
70 °C

실험 절차

0.27 g of acetonylacetone was added to a solution of 0.5 g of α-[2-chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetohydrazide (prepared as described in Example 13) dissolved in 5 ml of acetic acid, and the mixture was heated at 70° C. for 4 hours. The acetic acid used as the solvent was removed by evaporation under reduced pressure, and the residue was mixed with water to precipitate crystals. These crystals were collected by filtration, washed with water and dried. The product was purified by column chromatography through silica gel (eluent: a 98:2 by volume mixture of methylene chloride and ethanol), followed by recrystallization from ethanol to give 0.4 g of the title compound melting at 189°-190° C.

후처리

  1. customwas removed by evaporation under reduced pressure
  2. additionthe residue was mixed with water
  3. customto precipitate crystals
  4. filtrationThese crystals were collected by filtration
  5. washwashed with water
  6. customdried
  7. customThe product was purified by column chromatography through silica gel (eluent
  8. additiona 98:2 by volume mixture of methylene chloride and ethanol),
  9. customfollowed by recrystallization from ethanol

출처 및 근거

ORD 기록
ord-6cce6df8eceb465ab733904b7383fd67
출처 데이터셋
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04898862

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