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5-Chloro-6-nitro-1,1,3,3-tetrafluoro-1,3-dihydroisobenzofuran → 6-Amino-5-chloro-1,1,3,3-tetrafluoro-1,3-dihydroisobenzofuran

HRID 1871569
ノート
印刷プレビュー

反応式

HRID 1871569 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[N+:11]([O-])=O)[C:7]([F:15])([F:14])[O:6][C:5]2([F:17])[F:16]>C(O)(=O)C.O.[Fe]>[NH2:11][C:10]1[CH:9]=[C:8]2[C:4]([C:5]([F:17])([F:16])[O:6][C:7]2([F:14])[F:15])=[CH:3][C:2]=1[Cl:1]
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 1

HCID 157673125-Chloro-6-nitro-1,1,3,3-tetrafluoro-1,3-dihydroisobenzofuran

生成物 1

HCID 154773476-Amino-5-chloro-1,1,3,3-tetrafluoro-1,3-dihydroisobenzofuran収率 92.3%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

実験手順

To a solution wherein electrolytic iron powder (5.59 g, 100.0 mmol) is in acetic acid (100 ml) and water (10 ml), an acetic acid (20 ml) solution of 5-chloro-6-nitro-1,1,3,3-tetrafluoro-1,3-dihydroisobenzofuran (5.43 g, 20.0 mmol) was added dropwise at 50 to 60° C. over a period of about 10 minutes and further stirred for 30 minutes. The reaction solution was then filtered and water was poured into the filtrate. After the solution was extracted with ethyl acetate, the organic layer was washed with a saturated sodium hydrogencarbonate solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the residue was subjected to silica gel column chromatography to give 4.46 g of 6-amino-5-chloro-1,1,3,3-tetrafluoro-1,3-dihydroisobenzofuran.

後処理

  1. filtrationThe reaction solution was then filtered
  2. additionwater was poured into the filtrate
  3. extractionAfter the solution was extracted with ethyl acetate
  4. washthe organic layer was washed with a saturated sodium hydrogencarbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-020d298080384397b4a9956e492a3a75
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06103750

反応ノート

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