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

Sodium Carbonate → 2-(1H-indol-5-yl)-7-(morpholine-4-carbonyl)-5H-pyrido[3,2-b]indole-4-carboxamide

HRID 2410902
노트
인쇄 미리보기

반응식

HRID 2410902 반응식
Br[C:2]1[CH:3]=[C:4]([C:23]([NH2:25])=[O:24])[C:5]2[NH:6][C:7]3[CH:8]=[C:9]([C:15]([N:17]4[CH2:22][CH2:21][O:20][CH2:19][CH2:18]4)=[O:16])[CH:10]=[CH:11][C:12]=3[C:13]=2[N:14]=1.CC1(C)C(C)(C)OB([C:34]2[CH:35]=[C:36]3[C:40](=[CH:41][CH:42]=2)[NH:39][CH:38]=[CH:37]3)O1.[O-]P([O-])([O-])=O.[K+].[K+].[K+].C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.C([O-])([O-])=O.[Na+].[Na+]>CC([O-])=O.CC([O-])=O.[Pd+2].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CO.C1(C)C=CC=CC=1.C1COCC1>[NH:39]1[C:40]2[C:36](=[CH:35][C:34]([C:2]3[CH:3]=[C:4]([C:23]([NH2:25])=[O:24])[C:5]4[NH:6][C:7]5[CH:8]=[C:9]([C:15]([N:17]6[CH2:18][CH2:19][O:20][CH2:21][CH2:22]6)=[O:16])[CH:10]=[CH:11][C:12]=5[C:13]=4[N:14]=3)=[CH:42][CH:41]=2)[CH:37]=[CH:38]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 5

HCID 10340Sodium CarbonateHCID 62657Potassium Phosphate, TribasicHCID 27347725-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indoleHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 866630712-bromo-7-(morpholine-4-carbonyl)-5H-pyrido[3,2-b]indole-4-carboxamide

생성물 1

HCID 66604688
2-(1H-indol-5-yl)-7-(morpholine-4-carbonyl)-5H-pyrido[3,2-b]indole-4-carboxamide

시약·촉매·용매 5

HCID 167845palladium(II) acetate촉매HCID 178418397HCID 178418397, 화합물촉매HCID 887Methanol용매HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
85 °C

실험 절차

2-Bromo-7-(morpholine-4-carbonyl)-5H-pyrido[3,2-b]indole-4-carboxamide (60 mg, 0.149 mmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indole (72.3 mg, 0.298 mmol), Potassium phosphate tribasic (134 mg, 0.476 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl (24.43 mg, 0.060 mmol) and Pd(OAc)2 (6.68 mg, 0.030 mmol) were mixed with THF (2 mL) in a sealed microwave vial. The mixture was flushed with N2 and heated at 85° C. in an oil bath for 3.5 hr. LC/MS showed there was trace amount of product formed. The reaction mixture was blown to dryness under N2 blower. To the mixture was added Pd(Ph3P)4 (34.4 mg, 0.030 mmol), Toluene (3 mL), MeOH (1.5 mL) and Na2CO3 (2M) (0.149 mL, 0.298 mmol). The mixture was then heated at 100° C. for 3 hrs. The mixture was concentrated and purified using preparative HPLC to give titled product. MS (ESI) m/z 440.3 (M+H)+. 1H NMR (DMSO-d6) δ ppm 11.65 (s, 1H), 11.20 (s, 1H), 8.67 (s, 1H), 8.5 (m, 2H), 8.32 (d, 1H, J=8.2), 8.12 (d, 1H, J=8.5), 7.9 (s, 1H), 7.8 (s, 1H), 7.53(d, 1H, J=8.0), 7.41(m, 1H), 7.30 (d, 1H, J=8.0), 6.57 (s, 1H), 3.66 (bs, 8H).

후처리

  1. customThe mixture was flushed with N2
  2. customformed
  3. temperatureThe mixture was then heated at 100° C. for 3 hrs
  4. concentrationThe mixture was concentrated
  5. custompurified

출처 및 근거

ORD 기록
ord-6557ff14ff61491aaf6560c99c62f6be
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815840B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트