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Sodium Hydroxide → HCID 57675146, 화합물

HRID 490899
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HRID 490899 반응식
[OH-].[Na+].[CH2:3]([N:5]1[C:9]2=[N:10][CH:11]=[C:12]([C:22]([O:24]CC)=[O:23])[C:13]([N:14]([CH3:21])[CH:15]3[CH2:20][CH2:19][O:18][CH2:17][CH2:16]3)=[C:8]2[CH:7]=[N:6]1)[CH3:4]>C(O)C>[CH2:3]([N:5]1[C:9]2=[N:10][CH:11]=[C:12]([C:22]([OH:24])=[O:23])[C:13]([N:14]([CH3:21])[CH:15]3[CH2:20][CH2:19][O:18][CH2:17][CH2:16]3)=[C:8]2[CH:7]=[N:6]1)[CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 44561082Ethyl 1-ethyl-4-[methyl(tetrahydro-2H-pyran-4-yl)amino]-1H-pyrazolo[3,4-b]pyridine-5-carboxylate

생성물 1

HCID 57675146HCID 57675146, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
50 °C

실험 절차

Sodium hydroxide (0.43 g, 10.8 mmol) was added to a solution of Intermediate 51 in ethanol (10 ml, 95%). The reaction mixture was heated at 50° C. for 18 hours. The solvent was evaporated in vacuo and the residue dissolved in water and acidified to pH 3 by the addition of aqueous hydrochloric acid. The solution was extracted with DCM. The organic phase was separated using a hydrophobic frit (Whatman PTFE Folter Media with Polypropylene Housing 5 μM pore size) and the solvent evaporated in vacuo to give Intermediate 52 as a white solid (0.65 g). LCMS showed MH+=305; TRET=1.97 min.

후처리

  1. customThe solvent was evaporated in vacuo
  2. dissolutionthe residue dissolved in water
  3. additionacidified to pH 3 by the addition of aqueous hydrochloric acid
  4. extractionThe solution was extracted with DCM
  5. customThe organic phase was separated
  6. customthe solvent evaporated in vacuo

출처 및 근거

ORD 기록
ord-0d8a73ae84d1417992126827824f5ef2
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07528148B2

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