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Acetic Acid → 2-Amino-5-(4-fluorophenoxy)benzenethiol

HRID 359778
ノート
印刷プレビュー

反応式

HRID 359778 の反応式
NC1[S:3][C:4]2[CH:10]=[C:9]([O:11][C:12]3[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=3)[CH:8]=[CH:7][C:5]=2[N:6]=1.[OH-].[K+].C(O)(=O)C>O.C(O)CO>[NH2:6][C:5]1[CH:7]=[CH:8][C:9]([O:11][C:12]2[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=2)=[CH:10][C:4]=1[SH:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 219855122-Amino-6-(4-fluorophenoxy)benzothiazole

生成物 1

HCID 200638272-Amino-5-(4-fluorophenoxy)benzenethiol収率 80.5%

試薬・触媒・溶媒 2

HCID 174Ethylene Glycol溶媒HCID 962Water溶媒

実験手順

22 g of 2-amino-6-(4-fluorophenoxy)benzothiazole (prepared as described in preparation 7) were added to a mixture of a solution of 90 g of potassium hydroxide in 100 ml of water and 28 ml of ethylene glycol, and the mixture was stirred for 2 hours on an oil bath kept at 130° C under an atmosphere of nitrogen. After the mixture had been cooled to room temperature, 90 ml of acetic acid was added dropwise to the resulting homogenous solution to deposit a precipitate: this was extracted with toluene. The toluene extract was dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure, to afford 16 g of the title compound as a pale yellow solid.

後処理

  1. customkept at 130° C under an atmosphere of nitrogen
  2. extractionthis was extracted with toluene
  3. extractionThe toluene extract
  4. dry with materialwas dried over anhydrous magnesium sulfate
  5. concentrationconcentrated by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-e89974f932284d1380cde5ddab2d870f
出典データセット
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05002942

反応ノート

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