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

Sodium t-butoxide → HCID 178490933, 화합물

HRID 2239893
노트
인쇄 미리보기

반응식

HRID 2239893 반응식
Cl[C:2]1[CH:3]=[C:4]([N:19]([CH2:26][C:27]2[CH:32]=[CH:31][C:30]([O:33][CH3:34])=[CH:29][CH:28]=2)[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:5]2[N:6]([C:8]([CH:11]=[CH:12][C:13]3[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=3)=[CH:9][N:10]=2)[N:7]=1.C(N1CCCC(NC2C=C(N(CC3C=CC(OC)=CC=3)C3C=CC=CC=3)C3N(C(C#N)=CN=3)N=2)C1)C1C=CC=CC=1.CC(C)([O-])C.[Na+].[C@H:82]1([NH2:89])[CH2:87][CH2:86][C@H:85]([NH2:88])[CH2:84][CH2:83]1>CC(O)=O.CC(P(C(C)(C)C)C1C(C2[C-]=CC=CC=2)=CC=CC=1)(C)C.[Pd].C1(C)C=CC=CC=1>[NH2:88][C@H:85]1[CH2:86][CH2:87][C@H:82]([NH:89][C:2]2[CH:3]=[C:4]([N:19]([CH2:26][C:27]3[CH:32]=[CH:31][C:30]([O:33][CH3:34])=[CH:29][CH:28]=3)[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:5]3[N:6]([C:8]([CH:11]=[CH:12][C:13]4[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=4)=[CH:9][N:10]=3)[N:7]=2)[CH2:83][CH2:84]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 23676156Sodium t-butoxideHCID 68481210HCID 68481210, 화합물HCID 86618523HCID 86618523, 화합물HCID 178511674HCID 178511674, 화합물

생성물 1

HCID 178490933HCID 178490933, 화합물수율 38%

시약·촉매·용매 2

HCID 11982262
2-(2'-Di-tert-butylphosphine)biphenylpalladium(II) acetate
촉매
HCID 1140Toluene용매

반응 조건

온도
85 °C

실험 절차

6-chloro-N-(4-methoxybenzyl)-N-phenyl-3-(2-(pyridin-4-yl)vinyl)imidazo[1,2-b]pyridazin-8-amine (75 mg, 0.16 mmol) from (1b), sodium tert-butoxide (22 mg, 0.22 mmol), trans-1,4-cyclohexanediamine (22 mg, 0.19 mmol) and acetato(2′-di-tert-butylphosphino-1,1′-biphenyl-2-yl)palladium (II) (7.4 mg, 0.01 mmole) were purged with argon for 15 min. then toluene (0.6 mL) was added via syringe. The contents were sonicated briefly and heated at 85° C. for 2 h. After cooling to room temperature, the mixture was partitioned between EtOAc (200 mL) and water (20 mL), and the organic layer was washed with water, brine, dried over MgSO4 and concentrated. The residue was purified by reverse phase preparative HPLC to provide N6-(trans-4-aminocyclohexyl)-N8-(4-methoxybenzyl)-N8-phenyl-3-(2-(pyridin-4-yl)vinyl)imidazo[1,2-b]pyridazine-6,8-diamine as a yellow solid (32 mg, 38%). LCMS[M+H]+ 546.

후처리

  1. customThe contents were sonicated briefly
  2. temperatureAfter cooling to room temperature
  3. customthe mixture was partitioned between EtOAc (200 mL) and water (20 mL)
  4. washthe organic layer was washed with water, brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. customThe residue was purified by reverse phase preparative HPLC

출처 및 근거

ORD 기록
ord-24ae76a0eb804313bd1c0c0db8c8e96f
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07723336B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트