Potassium Carbonate → 6'-Ethynyl-2-fluoro-5-(4-piperidin-1-ylmethylphenyl)-[3,4']bipyridinyl-3'-ylamine

HRID 1888605노트

반응식

HRID 1888605 반응식
C[Si]([C:5]#[C:6][C:7]1[N:12]=[CH:11][C:10]([NH2:13])=[C:9]([C:14]2[C:15]([F:33])=[N:16][CH:17]=[C:18]([C:20]3[CH:25]=[CH:24][C:23]([CH2:26][N:27]4[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]4)=[CH:22][CH:21]=3)[CH:19]=2)[CH:8]=1)(C)C.C(=O)([O-])[O-].[K+].[K+]>CO.C(Cl)Cl>[C:6]([C:7]1[N:12]=[CH:11][C:10]([NH2:13])=[C:9]([C:14]2[C:15]([F:33])=[N:16][CH:17]=[C:18]([C:20]3[CH:21]=[CH:22][C:23]([CH2:26][N:27]4[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]4)=[CH:24][CH:25]=3)[CH:19]=2)[CH:8]=1)#[CH:5]

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 582665496'-((Trimethylsilyl)ethynyl)-2-fluoro-5-(4-piperidin-1-ylmethyl-phenyl)-[3,4']bipyridinyl-3'-ylamine

생성물 1

HCID 582664586'-Ethynyl-2-fluoro-5-(4-piperidin-1-ylmethylphenyl)-[3,4']bipyridinyl-3'-ylamine

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 6344Dichloromethane용매

실험 절차

A mixture of 6′-((trimethylsilyl)ethynyl)-2-fluoro-5-(4-piperidin-1-ylmethyl-phenyl)-[3,4′]bipyridinyl-3′-ylamine (90 mg, 0.2 mmol) and potassium carbonate (150 mg, 1.1 mmol) in methanol (2 mL) was stirred at ambient temperature for 1 h. The cooled reaction mixture was diluted with DCM (20 mL) and methanol (2 mL) and washed with water (15 mL). The organic phase was separated, dried over sodium sulfate, filtered and evaporated in vacuo to afford a brown residue that was taken to the next step without purification.

후처리

  1. customThe cooled reaction mixture
  2. washwashed with water (15 mL)
  3. customThe organic phase was separated
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customto afford a brown residue that
  8. customwas taken to the next step without purification

출처 및 근거

ORD 기록
ord-559c30819ed24f2aac128822fb0b8b33
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501765B2

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