Anisole → HCID 353540、化合物

HRID 905534ノート

反応式

HRID 905534 の反応式
C1(OC)C=CC=CC=1.[N+:9]([C:12]1[CH:28]=[CH:27][C:15]2[O:16][C:17]3[CH:23]=[C:22]([N+:24]([O-])=O)[CH:21]=[CH:20][C:18]=3[O:19][C:14]=2[CH:13]=1)([O-])=O.[H][H]>[Pd].C1COCC1>[NH2:24][C:22]1[CH:21]=[CH:20][C:18]2[O:19][C:14]3[CH:13]=[C:12]([NH2:9])[CH:28]=[CH:27][C:15]=3[O:16][C:17]=2[CH:23]=1

参加物

6

反応物 3

HCID 7519AnisoleHCID 1501562,7-Dinitrodibenzo-p-dioxinHCID 178418361HCID 178418361、化合物

生成物 1

HCID 353540HCID 353540、化合物収率 46.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 1200 ml of anisole and 800 ml of THF were added 69.7 g (0.254 mole) of 2,7-dinitrodibenzodioxin and 22.2 g of 10% palladium/carbon and hydrogen gas was passed through the mixture with stirring at room temperature for 8 hours. The 10% palladium/carbon was removed by filtration, then a precipitate containing the 10% palladium/carbon was collected by filtration, and the precipitate was rinsed with THF. The rinsings were concentrated and dried under reduced pressure to give 25.0 g (0.117 mole, 46.0% yield) of 2,7-diaminodibenzodioxin. The product showed a purity of 98.1% (HPLC, 254 nm).

後処理

  1. customThe 10% palladium/carbon was removed by filtration
  2. additiona precipitate containing the 10% palladium/carbon
  3. filtrationwas collected by filtration
  4. washthe precipitate was rinsed with THF
  5. concentrationThe rinsings were concentrated
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-21d6ba9caca04c3f9bbb3f352b77d03a
出典データセット
uspto-grants-2011_09
特許番号
US08012606B2

反応ノート

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