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HCID 19867711、化合物 → HCID 19867706、化合物

HRID 1198945
ノート
印刷プレビュー

反応式

HRID 1198945 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 19867711HCID 19867711、化合物

生成物 1

HCID 19867706HCID 19867706、化合物収率 38.4%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bd90a94980054809885b8800838e55c6
出典データセット
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04898872

反応ノート

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