Methanol → 2-[4-[1-[3-(Trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]phenoxy]acetic acid

HRID 2381117노트

반응식

HRID 2381117 반응식
O.[OH-].[Li+].[F:4][C:5]([F:35])([F:34])[C:6]1[N:10]2[N:11]=[C:12]([N:15]3[CH2:20][CH2:19][CH:18]([C:21]4[CH:33]=[CH:32][C:24]([O:25][CH2:26][C:27]([O:29]CC)=[O:28])=[CH:23][CH:22]=4)[CH2:17][CH2:16]3)[CH2:13][CH2:14][C:9]2=[N:8][N:7]=1.O.CO>C1COCC1>[F:35][C:5]([F:4])([F:34])[C:6]1[N:10]2[N:11]=[C:12]([N:15]3[CH2:20][CH2:19][CH:18]([C:21]4[CH:33]=[CH:32][C:24]([O:25][CH2:26][C:27]([OH:29])=[O:28])=[CH:23][CH:22]=4)[CH2:17][CH2:16]3)[CH2:13][CH2:14][C:9]2=[N:8][N:7]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 68503106Ethyl 2-[4-[1-[3-(trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]phenoxy]acetate

생성물 1

HCID 685023702-[4-[1-[3-(Trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]phenoxy]acetic acid수율 74.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Lithium hydroxide monohydrate (381 mg, 9.08 mmol) was added to ethyl 2-[4-[1-[3-(trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]phenoxy]acetate (820 mg, 1.82 mmol) in a mixture of THF (20 mL), water (10 mL) and MeOH (5 mL). The resulting mixture was stirred at ambient temperature for 16 hours. The solvents were evaporated then the residue was suspended in water and acidified to pH 4 with 1M citric acid. The resulting precipitate was collected by filtration, washed with water and dried to afford 2-[4-[1-[3-(trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]phenoxy]acetic acid (575 mg, 74.8%) as a solid.

후처리

  1. customThe solvents were evaporated
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-610ab451675f43808ec724f1479cab74
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258140B2

반응 노트

불러오는 중…