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Ethyl Acetate → HCID 21920030, 화합물

HRID 1244628
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반응식

HRID 1244628 반응식
[F:1][C:2]1[CH:18]=[CH:17][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][N:9]=2)=[CH:4][CH:3]=1.C(OCC)(=O)C>O.C(O)(=O)C.[Fe]>[F:1][C:2]1[CH:18]=[CH:17][C:5]([CH2:6][O:7][C:8]2[N:9]=[CH:10][C:11]([NH2:14])=[CH:12][CH:13]=2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 8857Ethyl AcetateHCID 21920020HCID 21920020, 화합물

생성물 1

HCID 21920030HCID 21920030, 화합물수율 45.8%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 176Acetic Acid용매HCID 962Water용매2회

실험 절차

A mixture of 0.70 g (2.8 mmol) of 2-(4-fluoro-benzyloxy)-5-nitro-pyridine and 2.36 g (4.2 mmol) of iron powder in 35 ml of water and 0.7 ml of acetic acid is heated under reflux for 4 hours. For the working-up, the reaction mixture is treated under vigorous stirring with water and ethyl acetate, thereafter, filtered over a layer of Dicalit. The organic layer is separated, dried over sodium sulfate and evaporated under reduced pressure. There are obtained 0.28 g (45% of theory) of 6-(4-fluoro-benzyloxy)-pyridin-3-ylamine as a greenish solid which is engaged in the next step without further purification.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 4 hours
  3. additionthe reaction mixture is treated
  4. filtrationfiltered over a layer of Dicalit
  5. customThe organic layer is separated
  6. dry with materialdried over sodium sulfate
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-8f9d9607702a451795268feb394e6d64
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07122562B2

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