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Ammonia → HCID 9856687、化合物

HRID 396951
ノート
印刷プレビュー

反応式

HRID 396951 の反応式
Cl[C:2]1[C:11]2[N:12]=[CH:13][N:14]([CH2:15][CH:16]([CH3:18])[CH3:17])[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1.CC1C([C:26]([OH:28])=O)=CC=CC=1.[NH3:29]>>[NH2:29][C:2]1[C:11]2[N:12]=[C:13]([CH2:26][OH:28])[N:14]([CH2:15][CH:16]([CH3:18])[CH3:17])[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 222AmmoniaHCID 88033762HCID 88033762、化合物

生成物 1

HCID 9856687HCID 9856687、化合物

反応条件

温度
175 °C

実験手順

4-Chloro-1-(2-methylpropyl)-1H-imidazo-[4,5-c]quinoline-2-methyl benzoate (5.0 g; 0.13 mol, Example 7) was added to 15% methanolic ammonia (50 mL). The mixture was heated in a Parr bomb for 7 hr at 175° C. The resulting solution was evaporated to reduce the volume. A sticky solid crystallized from the solution. The solid was filtered from the mixture and slurried in aqueous sodium bicarbonate solution. The resulting solid was filtered from the mixture, washed with water, and dried to yield 2.1 g (61.7%) of crude product which was recrystallized from ethanol several times to yield pure product m.p. 226-231° C. Analysis: Calculated: C, 66.6: H, 6.7; N, 20.7. Found: C, 66.4; H, 6.5; N, 20.4.

後処理

  1. customThe resulting solution was evaporated
  • customA sticky solid crystallized from the solution
  • filtrationThe solid was filtered from the mixture
  • filtrationThe resulting solid was filtered from the mixture
  • washwashed with water
  • customdried
  • customto yield 2.1 g (61.7%) of crude product which
  • customwas recrystallized from ethanol several times
  • 出典と根拠

    ORDレコード
    ord-599c52768b734fd3bdab3becfaef378c
    出典データセット
    uspto-grants-2003_08
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US06608201B2

    反応ノート

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