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

1,1,1-Trifluoro-2-propanamine → HCID 118271714, 화합물

HRID 590788
노트
인쇄 미리보기

반응식

HRID 590788 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]2[C:8](I)=[N:9][N:10]([C:11]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[C:4]=2[CH:3]=1.[F:31][C:32]([F:37])([F:36])[CH:33]([NH2:35])[CH3:34].CC(C)([O-])C.[Na+]>C1COCC1.CC(C1C=C(C(C)C)C(C2C(P(C(C)(C)C)C(C)(C)C)=CC=CC=2)=C(C(C)C)C=1)C.C1C=[C-]C(CCN)=CC=1.Cl[Pd+]>[Cl:1][C:2]1[N:7]=[CH:6][C:5]2[C:8]([NH:35][CH:33]([CH3:34])[C:32]([F:37])([F:36])[F:31])=[N:9][N:10]([C:11]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[C:4]=2[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 37831651,1,1-Trifluoro-2-propanamineHCID 23676156Sodium t-butoxideHCID 895258586-Chloro-3-iodo-1-trityl-1H-pyrazolo[4,3-c]pyridine

생성물 1

HCID 118271714HCID 118271714, 화합물수율 67%

시약·촉매·용매 2

HCID 92000389
Chloropalladium(1+) 2-(2-aminoethyl)benzen-1-ide--di-tert-butyl(2',4',6'-tri(propan-2-yl)(1,1'-biphenyl)-2-yl)phosphane (1/1/1)
촉매
HCID 8028Tetrahydrofuran용매

반응 조건

온도
80 °C

실험 절차

To a solution of 6-chloro-3-iodo-1-trityl-1H-pyrazolo[4,3-c]pyridine (0.5 g, 0.96 mmol) in anhydrous THF (5 mL) was added 1,1,1-trifluoropropan-2-amine (0.13 g, 1.2 mmol), t-Bu-X-Phos precatalyst (0.1 g, 0.14 mmol) and sodium-t-Butoxide (0.27 g, 2.8 mmol). The contents were heated to 80° C. in a sealed reaction vessel under inert atmosphere. After 4 h, the reaction mixture was brought back to ambient temperature, the reaction was quenched with H2O (10 mL) and the organic contents were extracted with EtOAc (2×50 mL), dried over Na2SO4 and concentrated. The residue thus obtained was purified by flash column chromatography, to afford the title compound (0.32 g, 67% yield). MS ESI calc'd. for C28H22ClF3N4 [M+H]+ 507. Found 507.

후처리

  1. customwas brought back to ambient temperature
  2. customthe reaction was quenched with H2O (10 mL)
  3. extractionthe organic contents were extracted with EtOAc (2×50 mL)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customThe residue thus obtained
  7. customwas purified by flash column chromatography

출처 및 근거

ORD 기록
ord-cd0222059da44893a9c04f9775b12627
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09233979B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트