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Trifluoroacetic acid → HCID 22492898, 화합물

HRID 1816351
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HRID 1816351 반응식
[CH:1]1([N:7]2[CH2:12][CH2:11][CH:10]([C:13]3[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[CH:15][CH:14]=3)[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.N[NH:22][C:23]([NH2:25])=[S:24].[F:26][C:27]([F:32])([F:31])[C:28]([OH:30])=[O:29]>C1(C)C=CC=CC=1>[F:26][C:27]([F:32])([F:31])[C:28]([OH:30])=[O:29].[CH:1]1([N:7]2[CH2:8][CH2:9][CH:10]([C:13]3[CH:14]=[CH:15][C:16]([C:17]4[S:24][C:23]([NH2:25])=[N:22][N:18]=4)=[CH:19][CH:20]=3)[CH2:11][CH2:12]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 2723789ThiosemicarbazideHCID 22492892HCID 22492892, 화합물

생성물 1

HCID 22492898HCID 22492898, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
70 °C

실험 절차

A mixture of 4-(1-cyclohexyl-4-piperidyl)benzonitrile (0.68 g), thiosemicarbazide (0.58 g) and trifluoroacetic acid (3.5 ml) in toluene (7 ml) was stirred for 7 hours at 70° C. After being cooled to room temperature, the solvent was evaporated in vacuo. Then the residue was dissolved in tetrahydrofuran and poured into water. The solution was adjusted to pH 8 with 1N aqueous sodium hydroxide. The resulting precipitate was collected by filtration and washed with water and isopropyl ether to give 5-[4-(1-cyclohexyl-4-piperidyl)phenyl]-1,3,4-thiadiazol-2-amine trifluroacetate (0.80 g).

후처리

  1. temperatureAfter being cooled to room temperature
  2. customthe solvent was evaporated in vacuo
  3. dissolutionThen the residue was dissolved in tetrahydrofuran
  4. additionpoured into water
  5. filtrationThe resulting precipitate was collected by filtration
  6. washwashed with water and isopropyl ether

출처 및 근거

ORD 기록
ord-a4cd9676a2ef4d1880f47db8c6c01c5c
출처 데이터셋
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06884774B2

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