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

HRID 1198902
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인쇄 미리보기

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HRID 1198902 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14](=[O:34])[CH2:15][O:16][C:17]2[CH:22]=[CH:21][C:20]([C:23](=O)[CH:24]([NH:26][C:27]([O:29]CC)=O)[CH3:25])=[CH:19][C:18]=2[Cl:33])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].O.[NH2:36][NH2:37]>C(O)CCC>[Cl:33][C:18]1[CH:19]=[C:20]([C:23]2[CH:24]([CH3:25])[NH:26][C:27](=[O:29])[NH:36][N:37]=2)[CH:21]=[CH:22][C:17]=1[O:16][CH2:15][C:14]([NH:13][CH2:12][CH2:11][C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)=[O:34]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 14370692N-[2-(3,4-Dimethoxyphenyl)ethyl]-alpha-{2-chloro-4-[2-(ethoxycarbonylamino)propionyl]phenoxy}acetamide

생성물 1

HCID 14370693alpha-[2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]-N-[2-(3,4-dimethoxyphenyl)ethyl]acetamide수율 21.5%

시약·촉매·용매 1

HCID 2631-Butanol용매2회

실험 절차

A mixture of 556 mg of N-[2-(3,4-dimethoxyphenyl)-ethyl]-α-{2-chloro-4-[2-(ethoxycarbonylamino)propionyl]phenoxy}acetamide [prepared as described in step (c) above] and 723 mg of hydrazine hydrate in 7 ml of butanol was heated under reflux for 67 hours. At the end of this time, the mixture was cooled, and the butanol used as the solvent was removed by evaporation under reduced pressure. The residue was purified by column chromatography through silica gel eluted with a 10:1 by volume mixture of chloroform and methanol, to give 112 mg of the title compound as a white powder melting at 167°-169° C. (with decomposition).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 67 hours
  3. temperatureAt the end of this time, the mixture was cooled
  4. customwas removed by evaporation under reduced pressure
  5. customThe residue was purified by column chromatography through silica gel
  6. washeluted with a 10:1 by volume mixture of chloroform and methanol

출처 및 근거

ORD 기록
ord-1f53aa30cbd04b579494b97b450a5dea
출처 데이터셋
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04898862

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