홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Cesium carbonate → 6-Trifluoromethyl-pyridine-2-carboxylic acid[6-(4-tert-butylcarbamoyl-piperidin-1-ylmethyl)-pyrimidin-4-yl]-amide

HRID 1486749
노트
인쇄 미리보기

반응식

HRID 1486749 반응식
[C:1]([NH:5][C:6]([CH:8]1[CH2:13][CH2:12][N:11]([CH2:14][B-](F)(F)F)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl[C:20]1[N:25]=[CH:24][N:23]=[C:22]([NH:26][C:27]([C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([C:35]([F:38])([F:37])[F:36])[N:30]=2)=[O:28])[CH:21]=1.CC(C1C=C(C(C)C)C(C2C=CC=CC=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C.C([O-])([O-])=O.[Cs+].[Cs+]>C1COCC1.O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[C:1]([NH:5][C:6]([CH:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:20]2[N:25]=[CH:24][N:23]=[C:22]([NH:26][C:27]([C:29]3[CH:34]=[CH:33][CH:32]=[C:31]([C:35]([F:36])([F:38])[F:37])[N:30]=3)=[O:28])[CH:21]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10796Cesium carbonateHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl2회HCID 867065656-Trifluoromethyl-pyridine-2-carboxylic acid (6-chloro-pyrimidin-4-yl)-amideHCID 131736817((4-(Tert-butylcarbamoyl)piperidin-1-yl)methyl)trifluoroborate

생성물 1

HCID 118521926
6-Trifluoromethyl-pyridine-2-carboxylic acid[6-(4-tert-butylcarbamoyl-piperidin-1-ylmethyl)-pyrimidin-4-yl]-amide

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 21881883Oxolane--water (1/1)용매

반응 조건

온도
80 °C

실험 절차

To a solution of ((4-(tert-butylcarbamoyl)piperidin-1-yl)methyl)trifluoroborate (45 mg, 0.169 mmol) in THF/water 4:1 (3 mL) are added 6-trifluoromethyl-pyridine-2-carboxylic acid (6-chloro-pyrimidin-4-yl)-amide (51.2 mg, 0.169 mmol), palladium (II) acetate, (0.949 mg, 0.00423 mmol,), X-Phos, (2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl) (4.84 mg, 0.0101 mmol) and Cs2CO3, (165 mg, 0.507 mmol). The mixture is purged with argon and is stirred overnight in a sealed tube at 80° C. The mixture is let to cool down. Water (3 mL) and AcOEt (5 mL) are added and the aqueous phase is extracted with AcOEt (10 mL). The organic phase is dried over MgSO4, filtered and evaporated. The residue is purified by prep HPLC E delivering the title compound (27 mg, 30%) as a white powder, LC-MS A: tR=0.74 min; [M+H]+=465.4.

후처리

  1. customThe mixture is purged with argon
  2. temperatureto cool down
  3. additionWater (3 mL) and AcOEt (5 mL) are added
  4. extractionthe aqueous phase is extracted with AcOEt (10 mL)
  5. dry with materialThe organic phase is dried over MgSO4
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue is purified by prep HPLC E

출처 및 근거

ORD 기록
ord-7a928ac18881410ab4577b4524703fce
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09428456B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트