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Sodium Hydroxide → [6-[3-[4-(Diphenylmethoxy)piperidino]propylamino][1,2,4]triazolo[1,5-b]pyridazin-7-yl]carboxylic acid

HRID 1169101
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HRID 1169101 반응식
[C:1]1([CH:7]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[O:8][CH:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][NH:18][C:19]3[C:20]([C:28]([O:30]C)=[O:29])=[CH:21][C:22]4[N:23]([N:25]=[CH:26][N:27]=4)[N:24]=3)[CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+]>C(O)C>[C:32]1([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[O:8][CH:9]2[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:17][NH:18][C:19]3[C:20]([C:28]([OH:30])=[O:29])=[CH:21][C:22]4[N:23]([N:25]=[CH:26][N:27]=4)[N:24]=3)[CH2:13][CH2:14]2)[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 53760718Methyl [6-[3-[4-(diphenylmethoxy)piperidino]propylamino][1,2,4]triazolo[1,5-b]pyridazin-7-yl]carboxylate

생성물 1

HCID 22989252[6-[3-[4-(Diphenylmethoxy)piperidino]propylamino][1,2,4]triazolo[1,5-b]pyridazin-7-yl]carboxylic acid수율 51.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.58 g of methyl [6-[3-[4-(diphenylmethoxy)piperidino]propylamino][1,2,4]triazolo[1,5-b]pyridazin-7-yl]carboxylate was dissolved in 10 ml of ethanol; 8.0 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by stirring at room temperature for 1.5 hours. After cooling, the mixture was concentrated under reduced pressure. The residue was diluted with water and washed with ethyl acetate; 1N hydrochloric acid was added to adjust pH 4.5. The mixture was saturated with saline and extracted with tetrahydrofuran; the extract was dried over magnesium sulfate. The crystal obtained by concentration under reduced pressure was washed with ethyl ether, collected by filtration and dried to yield 788 mg of the title compound.

후처리

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated under reduced pressure
  3. additionThe residue was diluted with water
  4. washwashed with ethyl acetate
  5. addition1N hydrochloric acid was added
  6. extractionextracted with tetrahydrofuran
  7. dry with materialthe extract was dried over magnesium sulfate
  8. customThe crystal obtained by concentration under reduced pressure
  9. washwas washed with ethyl ether
  10. filtrationcollected by filtration
  11. customdried

출처 및 근거

ORD 기록
ord-bba2248a4b2549e5bd9d38dcb21f923c
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06627630B1

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