Lithium hydroxide, monohydrate → 4-[1-[3-(Trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoic acid

HRID 1675090노트

반응식

HRID 1675090 반응식
O.[OH-].[Li+].[F:4][C:5]([F:32])([F:31])[C:6]1[N:10]2[N:11]=[C:12]([N:15]3[CH2:20][CH2:19][CH:18]([C:21]4[CH:30]=[CH:29][C:24]([C:25]([O:27]C)=[O:26])=[CH:23][CH:22]=4)[CH2:17][CH2:16]3)[CH:13]=[CH:14][C:9]2=[N:8][N:7]=1>CO.O>[F:32][C:5]([F:4])([F:31])[C:6]1[N:10]2[N:11]=[C:12]([N:15]3[CH2:20][CH2:19][CH:18]([C:21]4[CH:30]=[CH:29][C:24]([C:25]([OH:27])=[O:26])=[CH:23][CH:22]=4)[CH2:17][CH2:16]3)[CH:13]=[CH:14][C:9]2=[N:8][N:7]=1

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 67340080Methyl 4-[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoate

생성물 1

HCID 673391044-[1-[3-(Trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoic acid수율 97%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

Lithium hydroxide monohydrate (0.154 g, 3.66 mmol) was added to methyl 4-[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoate (1.35 g, 3.33 mmol) in a mixture of methanol (30 mL) and water (15 mL). The resulting suspension was stirred at 50° C. for 16 hours. The mixture was cooled to room temperature, the methanol evaporated and the aqueous residue treated with 1M citric acid until precipitation ceased. The precipitate was collected by filtration, washed with water and dried to give 4-[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoic acid (1.26 g, 97%) as a solid.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. customthe methanol evaporated
  3. additionthe aqueous residue treated with 1M citric acid until precipitation
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-176b20c597394fbe8dfe6d92c73707fb
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003649B2

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