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Acetic Anhydride → HCID 21874908、化合物

HRID 2110408
ノート
印刷プレビュー

反応式

HRID 2110408 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 217302841-Fluoro-5-nitronaphthalene

生成物 1

HCID 21874908HCID 21874908、化合物収率 97%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

実験手順

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.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-80e208294d3944009a0fda65557d77f2
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07517904B2

反応ノート

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