4-(Trifluoromethoxy)benzoic acid hydrazide → HCID 178516246, 화합물

HRID 387451노트

반응식

HRID 387451 반응식
[F:1][C:2]([F:15])([F:14])[O:3][C:4]1[CH:13]=[CH:12][C:7]([C:8]([NH:10][NH2:11])=O)=[CH:6][CH:5]=1.I.CS[C:19](=[NH:28])[NH:20][C:21]1[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=1>N1C=CC=CC=1>[F:1][C:2]([F:15])([F:14])[O:3][C:4]1[CH:13]=[CH:12][C:7]([C:8]2[NH:28][C:19]([NH:20][C:21]3[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=3)=[N:11][N:10]=2)=[CH:6][CH:5]=1

참가 물질

4

반응물 2

HCID 27772304-(Trifluoromethoxy)benzoic acid hydrazideHCID 178504017HCID 178504017, 화합물

생성물 1

HCID 178516246HCID 178516246, 화합물수율 40.7%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

4-trifluoromethoxybenzoic acid hydrazide (1.1 g, 5.0 mmol) and S-methyl N-[4-hydroxy-phenyl]isothiourea hydroiodide (1.55 g, 5.0 mmol) were suspended in 10 mL of anhydrous pyridine. The reaction mixture was refluxed for 24 hours, during which time it changed color from yellow into orange-red. Then it was cooled down to ambient temperature and poured with stirring into 150 mL of ice-water. The aqueous layer was decanted and the resulting residue was purified by silica gel chromatography using 1:1 mixture of ethyl acetate/hexane. Solvent was removed in vacuo to give the title product as a pinkish-grey solid (684.0 mg). 40.6% yield.

후처리

  1. temperatureThe reaction mixture was refluxed for 24 hours, during which time it
  2. additionpoured
  3. customThe aqueous layer was decanted
  4. customthe resulting residue was purified by silica gel chromatography
  5. addition1:1 mixture of ethyl acetate/hexane
  6. customSolvent was removed in vacuo

출처 및 근거

ORD 기록
ord-b6dbb7ea7e3445c9bd39fbadf17acb60
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372971B2

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