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

HRID 1169104노트

반응식

HRID 1169104 반응식
C([O:4][C:5]([C:7]1[N:15]=[C:14]2[N:9]([N:10]=[C:11]([O:16][CH2:17][CH2:18][CH2:19][N:20]3[CH2:25][CH2:24][CH:23]([O:26][CH:27]([C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)[C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[CH2:22][CH2:21]3)[CH:12]=[CH:13]2)[N:8]=1)=[O:6])(C)C.[OH-].[Na+]>O1CCCC1>[C:34]1([CH:27]([C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)[O:26][CH:23]2[CH2:24][CH2:25][N:20]([CH2:19][CH2:18][CH2:17][O:16][C:11]3[CH:12]=[CH:13][C:14]4[N:9]([N:8]=[C:7]([C:5]([OH:6])=[O:4])[N:15]=4)[N:10]=3)[CH2:21][CH2:22]2)[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 53847838Isopropyl [6-[3-[4-(diphenylmethoxy) piperidino]propoxy][1,2,4]triazolo[1,5-b]pyridazin-2-yl]carboxylate

생성물 1

HCID 22989225[6-[3-[4-(Diphenylmethoxy)piperidino]propoxy][1,2,4]triazolo[1,5-b]pyridazin-2-yl]carboxylic acid수율 78.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1.85 g of isopropyl[6-[3-[4-(diphenylmethoxy)piperidino]propoxy][1,2,4]triazolo[1,5-b]pyridazin-2-yl]carboxylate was dissolved in 18 ml of tetrahydrofuran; 3.8 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by stirring at room temperature for 3.5 hours. After cooling, the mixture was concentrated under reduced pressure. The residue was diluted with water and washed with ethyl acetate; 1 N hydrochloric acid was added to adjust pH 4.5. The mixture was crystallized by the addition of ethanol-acetone (1:2), collected by filtration, washed with water and ethyl acetate and dried to yield 1.33 g 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. addition1 N hydrochloric acid was added
  6. customThe mixture was crystallized by the addition of ethanol-acetone (1:2)
  7. filtrationcollected by filtration
  8. washwashed with water and ethyl acetate
  9. customdried

출처 및 근거

ORD 기록
ord-8779ebb16c324e6d8acfd9f938daeef6
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06627630B1

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