Water → HCID 12445399, 화합물

HRID 240358

반응식

HRID 240358 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][C:11]1[CH:19]=[CH:18][C:14]2[O:15][CH2:16][O:17][C:13]=2[CH:12]=1)([O-])=O.C(OCC)(=O)C.O>[Fe].C(O)(=O)C>[O:15]1[C:14]2[CH:18]=[CH:19][C:11]([NH:10][C:5]3[C:4]([NH2:1])=[CH:9][CH:8]=[CH:7][CH:6]=3)=[CH:12][C:13]=2[O:17][CH2:16]1

참가 물질

6

반응물 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 7922985N-(2-nitrophenyl)benzo[d][1,3]dioxol-5-ylamine

생성물 1

HCID 12445399HCID 12445399, 화합물수율 100.8%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

반응 조건

온도
70 °C

실험 절차

13.6 g (244 mmol) of iron powder and 10.5 g (40 mmol) of N-(2-nitrophenyl)benzo[d][1,3]dioxol-5-ylamine were added to a solvent mixture of ethyl acetate (130 ml), water (65 mL) and acetic acid (15 mL), and the mixture was stirred for 1 hour at 70° C. The reaction solution was cooled to room temperature, and the waste was separated by filtration using a filter aid. The organic layer of the filtrate was batched off, washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 9.2 g (yield: 99%) of N-(benzo[d][1,3]dioxol-5-yl)benzene-1,2-diamine as white crystals.

후처리

  1. temperatureThe reaction solution was cooled to room temperature
  2. customthe waste was separated by filtration
  3. washwashed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3dcdf96401424292ba6f3b0c12a2ef12
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648075B2

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