Stannous chloride dihydrate → 2-(2,4-Dimethylphenoxy)-1,3-benzothiazol-7-amine

HRID 2235504ノート

反応式

HRID 2235504 の反応式
[CH3:1][C:2]1[CH:20]=[C:19]([CH3:21])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[S:6][C:7]2[C:13]([N+:14]([O-])=O)=[CH:12][CH:11]=[CH:10][C:8]=2[N:9]=1.O.O.[Sn](Cl)Cl>CN(C=O)C.C([O-])(O)=O.[Na+]>[CH3:1][C:2]1[CH:20]=[C:19]([CH3:21])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[S:6][C:7]2[C:13]([NH2:14])=[CH:12][CH:11]=[CH:10][C:8]=2[N:9]=1

参加物

5

反応物 2

HCID 61436Stannous chloride dihydrateHCID 685813382-(2,4-Dimethylphenoxy)-7-nitro-1,3-benzothiazole

生成物 1

HCID 685813992-(2,4-Dimethylphenoxy)-1,3-benzothiazol-7-amine収率 114%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
80 °C

実験手順

A mixture of 2-(2,4-dimethylphenoxy)-7-nitro-1,3-benzothiazole (220 mg, 0.733 mmol) and tin(II) chloride dihydrate (694 mg, 3.66 mmol) in DMF (10 ml) was stirred at 80° C. for 15 h and diluted with saturated NaHCO3 solution. The aqueous solution was extracted with AcOEt. The extract was washed with brine, dried over Magnesium sulfate, and concentrated under vacuum. The residue was purified by chromatography eluting with 10% AcOEt in n-hexane to afford 226 mg of the title compound.

後処理

  1. extractionThe aqueous solution was extracted with AcOEt
  2. washThe extract was washed with brine
  3. dry with materialdried over Magnesium sulfate
  4. concentrationconcentrated under vacuum
  5. customThe residue was purified by chromatography
  6. washeluting with 10% AcOEt in n-hexane

出典と根拠

ORDレコード
ord-460d428c2de7416b8b49efe3904bb172
出典データセット
uspto-grants-2010_05
特許番号
US07714009B2

反応ノート

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