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Acetic Anhydride → HCID 21874908, 화합물

HRID 2110408
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HRID 2110408 반응식
[F:1][C:2]1[C:11]2[C:6](=[C:7]([N+:12]([O-])=O)[CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1.[CH3:15][C:16](OC(C)=O)=[O:17]>CC(O)=O.[Fe]>[F:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[CH:10]=[CH:9][CH:8]=[C:7]2[NH:12][C:16](=[O:17])[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 7918Acetic AnhydrideHCID 217302841-Fluoro-5-nitronaphthalene

생성물 1

HCID 21874908HCID 21874908, 화합물수율 97%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

실험 절차

A solution of 141 mg (0.74 mmol) of compound 208A in 2 mL of AcOH was heated to reflux and treated with small portions of iron powder (118 mg, 2.11 mmol). The mixture was kept at reflux for 15 min before 73 μL (0.78 mmol) of Ac2O was added. After an additional 15 min at reflux, the mixture was cooled and filtered eluting with CH2Cl2. The filtrate was then concentrated under reduced pressure and the residue was purified by flash chromatography on silica gel eluting with 20 to 50% EtOAc in to give 145 mg (0.71 mmol, 97%) of compound 209A as a white solid.

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후처리

  1. temperatureto reflux
  2. additionwas added
  3. temperatureAfter an additional 15 min at reflux
  4. temperaturethe mixture was cooled
  5. filtrationfiltered
  6. washeluting with CH2Cl2
  7. concentrationThe filtrate was then concentrated under reduced pressure
  8. customthe residue was purified by flash chromatography on silica gel eluting with 20 to 50% EtOAc in

출처 및 근거

ORD 기록
ord-80e208294d3944009a0fda65557d77f2
출처 데이터셋
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07517904B2

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