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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Anhydride → HCID 53358059, 화합물

HRID 1500774
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HRID 1500774 반응식
C(N(CC)CC)C.C(O[C:12](=[O:14])[CH3:13])(=O)C.[NH:15]1[CH2:20][CH2:19][CH2:18][C@@H:17]([NH:21][C:22]2[CH:27]=[CH:26][N:25]=[C:24]([C:28]3[CH:29]=[N:30][N:31]4[CH:36]=[CH:35][C:34]([C:37]#[N:38])=[CH:33][C:32]=34)[N:23]=2)[CH2:16]1>CN(C)C1C=CN=CC=1.ClCCl>[C:12]([N:15]1[CH2:20][CH2:19][CH2:18][C@@H:17]([NH:21][C:22]2[CH:27]=[CH:26][N:25]=[C:24]([C:28]3[CH:29]=[N:30][N:31]4[CH:36]=[CH:35][C:34]([C:37]#[N:38])=[CH:33][C:32]=34)[N:23]=2)[CH2:16]1)(=[O:14])[CH3:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 67327163HCID 67327163, 화합물

생성물 1

HCID 53358059HCID 53358059, 화합물수율 46.1%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

Triethylamine (44 μL, 0.32 mmol), acetic anhydride (8.2 μL, 0.09 mmol) and N,N-dimethylpyridin-4-amine (1.2 mg, 0.01 mmol) were added to a stirred solution of 3-{4-[(3R)-piperidin-3-ylamino]pyrimidin-2-yl}pyrazolo[1,5-a]pyridine-5-carbonitrile (Preparation 7b, 40 mg, 0.06 mmol) in dichloromethane (1.5 mL) and the mixture was stirred at ambient temperature for 20 hours before being partitioned between dichloromethane and 4% aqueous sodium hydrogen carbonate solution. The organic layer was separated, washed with water and brine, dried (MgSO4) and the solvent was evaporated in vacuo. The crude product was purified by flash chromatography (100:1 to 20:1 chloroform/methanol) to give the title compound (10 mg, 44%) as a solid.

후처리

  1. custombefore being partitioned between dichloromethane and 4% aqueous sodium hydrogen carbonate solution
  2. customThe organic layer was separated
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. customthe solvent was evaporated in vacuo
  6. customThe crude product was purified by flash chromatography (100:1 to 20:1 chloroform/methanol)

출처 및 근거

ORD 기록
ord-4620420933a644659bfeaf6534d0c69e
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09206183B2

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