Water → 13-Amino-6-methoxy-3,3,14-trimethyl-3,14-dihydro-7H-benzo[b]pyrano-[3,2-h]acridin-7-one

HRID 1827908ノート

反応式

HRID 1827908 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[O:29][C:28]([CH3:31])([CH3:30])[CH:27]=[CH:26][C:6]2=[C:7]2[C:16]=1[C:15](=[O:17])[C:14]1[CH:13]=[C:12]3[CH:18]=[CH:19][CH:20]=[CH:21][C:11]3=[C:10]([N+:22]([O-])=O)[C:9]=1[N:8]2[CH3:25].O>C(O)(=O)C.[Zn]>[NH2:22][C:10]1[C:9]2[N:8]([CH3:25])[C:7]3[C:16](=[C:3]([O:2][CH3:1])[CH:4]=[C:5]4[O:29][C:28]([CH3:30])([CH3:31])[CH:27]=[CH:26][C:6]4=3)[C:15](=[O:17])[C:14]=2[CH:13]=[C:12]2[CH:18]=[CH:19][CH:20]=[CH:21][C:11]=12

参加物

5

反応物 2

HCID 962WaterHCID 220645286-Methoxy-3,3,14-trimethyl-13-nitro-3,14-dihydro-7H-benzo[b]pyrano-[3,2-h]acridin-7-one

生成物 1

HCID 1023744413-Amino-6-methoxy-3,3,14-trimethyl-3,14-dihydro-7H-benzo[b]pyrano-[3,2-h]acridin-7-one

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

実験手順

To 178 mg of the compound obtained in Step 6 above in 10 ml of acetic acid and 1 ml of water there are added 621 mg of zinc wool. The reaction mixture is stirred at ambient temperature for 2.5 hours and is then filtered. The filtrate is made alkaline using 10% aqueous ammonium hydroxide solution; the precipitate formed is then separated off by filtration. The crude residue is purified by chromatography over silica gel (dichloromethane/methanol: gradient from 0.1 to 0.5%), allowing the expected product to be isolated.

後処理

  1. filtrationis then filtered
  2. customthe precipitate formed
  3. customis then separated off by filtration
  4. customThe crude residue is purified by chromatography over silica gel (dichloromethane/methanol: gradient from 0.1 to 0.5%)
  5. customto be isolated

出典と根拠

ORDレコード
ord-cb64f6c53ae24b8bb36df999cc3e1cad
出典データセット
uspto-grants-2006_06
特許番号
US07056929B2

反応ノート

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