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Hydrazine hydrate (1:1) → HCID 178418252、化合物

HRID 1598619
ノート
印刷プレビュー

反応式

HRID 1598619 の反応式
[Br:1][C:2]1[CH:11]=[C:10]([CH2:12][CH3:13])[CH:9]=[C:8]2[C:3]=1[C:4]([OH:22])=[C:5]([C:18](OC)=[O:19])[C:6]([C:14](OC)=[O:15])=[N:7]2.O.[NH2:24][NH2:25]>C(O)C>[Br:1][C:2]1[C:3]2[C:4]([OH:22])=[C:5]3[C:18](=[O:19])[NH:25][NH:24][C:14](=[O:15])[C:6]3=[N:7][C:8]=2[CH:9]=[C:10]([CH2:12][CH3:13])[CH:11]=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 2

HCID 24654Hydrazine hydrate (1:1)HCID 178435441HCID 178435441、化合物

生成物 1

HCID 178418252HCID 178418252、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a mixture of dimethyl 5-bromo-7-ethyl-4-hydroxyquinoline-2,3-dicarboxylate (1.0 g, 2.7 mM,) in ethanol (25 mL) was added hydrazine hydrate (0.68 g, 14 mM). The resulting mixture was concentrated at 30° C. using a rotary evaporator and the residue was diluted with another portion of ethanol (25 mL) and similarly concentrated at 30° C. The residue was suspended in ethanol and filtered to separate the title compound (0.82 g, 82%) as a light yellow solid. Recrystallization of a portion of this material from dimethylsulfoxide/ethanol provided an analytical sample of the title compound as a light yellow crystalline solid, mp 335°-340° C. (dec).

後処理

  1. concentrationThe resulting mixture was concentrated at 30° C.
  2. customa rotary evaporator
  3. additionthe residue was diluted with another portion of ethanol (25 mL)
  4. concentrationsimilarly concentrated at 30° C
  5. filtrationfiltered
  6. customto separate the title compound (0.82 g, 82%) as a light yellow solid
  7. customRecrystallization of a portion of this material from dimethylsulfoxide/ethanol

出典と根拠

ORDレコード
ord-e633bd7d423d423c8f4da9d279257242
出典データセット
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05739133

反応ノート

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