Hydrochloric Acid → HCID 15219197、化合物

HRID 889240ノート

反応式

HRID 889240 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[C:10]=1[N+:16]([O-])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[Sn]Cl.Cl>CCO>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[C:10]=1[NH2:16])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24479Stannous ChlorideHCID 578349821-(Benzyloxy)-3-fluoro-2-nitrobenzene

生成物 1

HCID 15219197HCID 15219197、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1-benzyloxy-3-fluoro-2-nitrobenzene (1.32 g, 5.34 mmol), SnCl2 (4.96 g, 26.2 mmol), and 1N HCl (5.5 mL, 5.5 mmol) in EtOH (25 mL) is refluxed for 18 h. The mixture is concentrated and stirred with EtOAc and 1N NaOH solution. Solid NaOH is added until strongly basic. The precipitate is removed by filtration, and the organic phase is separated. It is then dried and concentrated. The residue is purified to give the title compound: MS (M+H)+=218.

後処理

  1. temperatureis refluxed for 18 h
  2. concentrationThe mixture is concentrated
  3. additionSolid NaOH is added until strongly basic
  4. customThe precipitate is removed by filtration
  5. customthe organic phase is separated
  6. customIt is then dried
  7. concentrationconcentrated
  8. customThe residue is purified

出典と根拠

ORDレコード
ord-c9200f16d57a49a9be17e27aa34bd76d
出典データセット
uspto-grants-2012_08
特許番号
US08252820B2

反応ノート

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