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

HRID 1827908노트

반응식

HRID 1827908 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cb64f6c53ae24b8bb36df999cc3e1cad
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07056929B2

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