Sodium Hydroxide → 2-[3-Chloro-6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionic Acid

HRID 1067540노트

반응식

HRID 1067540 반응식
Cl.Cl.[Cl:3][C:4]1[N:8]2[N:9]=[C:10]([NH:13][CH2:14][CH2:15][CH2:16][N:17]3[CH2:22][CH2:21][CH:20]([O:23][CH:24]([C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)[C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)[CH2:19][CH2:18]3)[CH:11]=[CH:12][C:7]2=[N:6][C:5]=1[C:37]([CH3:44])([CH3:43])[C:38]([O:40]CC)=[O:39].[OH-].[Na+]>C(O)C>[Cl:3][C:4]1[N:8]2[N:9]=[C:10]([NH:13][CH2:14][CH2:15][CH2:16][N:17]3[CH2:18][CH2:19][CH:20]([O:23][CH:24]([C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=4)[C:31]4[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=4)[CH2:21][CH2:22]3)[CH:11]=[CH:12][C:7]2=[N:6][C:5]=1[C:37]([CH3:44])([CH3:43])[C:38]([OH:40])=[O:39]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22989228Ethyl 2-[3-chloro-6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate dihydrochloride

생성물 1

HCID 229893252-[3-Chloro-6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionic Acid수율 84%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

653 mg of ethyl 2-[3-chloro-6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate dihydrochloride was dissolved in 6 ml of ethanol; 1.97 ml of a 2 N aqueous solution of sodium hydroxide was added, followed by thermal refluxing for 2.5 hours. After cooling, the mixture was concentrated under reduced pressure; the residue was diluted with water and washed with ethyl acetate; the water layer was ajusted to pH 4.5 by the addition of 1 N hydrochloric acid. Acetone was added; the crystal precipitated was collected by filtration, washed with water-acetone (5:1) and dried to yield 465 mg of the title compound.

후처리

  1. customrefluxing for 2.5 hours
  2. temperatureAfter cooling
  3. concentrationthe mixture was concentrated under reduced pressure
  4. additionthe residue was diluted with water
  5. washwashed with ethyl acetate
  6. additionthe water layer was ajusted to pH 4.5 by the addition of 1 N hydrochloric acid
  7. additionAcetone was added
  8. customthe crystal precipitated
  9. filtrationwas collected by filtration
  10. washwashed with water-acetone (5:1)
  11. customdried

출처 및 근거

ORD 기록
ord-8f60ff744ea749948c03fdefb544d6eb
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248740B1

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