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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 19867711, 화합물 → HCID 19867706, 화합물

HRID 1198945
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HRID 1198945 반응식
[CH3:1][C:2]1([CH3:17])[C:11]2[C:6](=[C:7]([CH3:15])[CH:8]=[C:9]([N+:12]([O-])=O)[CH:10]=2)[NH:5][C:4](=[O:16])[CH2:3]1>C(O)C.[Ni]>[CH3:1][C:2]1([CH3:17])[C:11]2[C:6](=[C:7]([CH3:15])[CH:8]=[C:9]([NH2:12])[CH:10]=2)[NH:5][C:4](=[O:16])[CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 19867711HCID 19867711, 화합물

생성물 1

HCID 19867706HCID 19867706, 화합물수율 38.4%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

A solution of 3,4-dihydro-4,4-dimethyl-6-nitro-8-methyl-2-(1H)-quinolone (9.46 g) in absolute ethanol (80 cm3) was hydrogenated at 60° and 60 p.s.i. (4.13×105Pa) pressure over Raney nickel (0.9 g) for 6 hours. The cooled solution was then filtered through "Solkafloc" (Trade mark for a cellulose based filtering aid) and evaporated in vacuo to give a solid which was chromatographed on silica (Merck "MK 60.9385" [Trade Mark]) eluting with methanol:chloroform, 1:33 by volume. Combination and evaporation of appropriate fractions gave the title compound (3.17 g) which was characterised spectroscopically and used directly in Preparation 22 without further purification.

후처리

  1. customwas hydrogenated at 60°
  2. filtrationThe cooled solution was then filtered through "Solkafloc" (Trade mark for a cellulose
  3. filtrationbased filtering aid) and
  4. customevaporated in vacuo
  5. customto give a solid which
  6. customwas chromatographed on silica (Merck "MK 60.9385" [Trade Mark])
  7. washeluting with methanol
  8. customCombination and evaporation of appropriate fractions

출처 및 근거

ORD 기록
ord-bd90a94980054809885b8800838e55c6
출처 데이터셋
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04898872

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