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

HRID 359778
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반응식

HRID 359778 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 200638272-Amino-5-(4-fluorophenoxy)benzenethiol수율 80.5%

시약·촉매·용매 2

HCID 174Ethylene Glycol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e89974f932284d1380cde5ddab2d870f
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05002942

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