Anisole → HCID 353540, 화합물

HRID 905534노트

반응식

HRID 905534 반응식
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

참가 물질

6

반응물 3

HCID 7519AnisoleHCID 1501562,7-Dinitrodibenzo-p-dioxinHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 353540HCID 353540, 화합물수율 46.1%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-21d6ba9caca04c3f9bbb3f352b77d03a
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012606B2

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