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

1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → N-(2-(5-(3,4-dichlorophenyl)furan-2-yl)ethyl)-3-(pyridin-4-yl)-1H-pyrazole-5-carboxamide

HRID 872454
노트
인쇄 미리보기

반응식

HRID 872454 반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[CH2:8][C:9]([C:12]([OH:14])=O)=[N:10][N:11]=2)=[CH:3][CH:2]=1.CCN(C(C)C)C(C)C.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.Cl.[Cl:46][C:47]1[CH:48]=[C:49]([C:54]2[O:58][C:57]([CH2:59][CH2:60][NH2:61])=[CH:56][CH:55]=2)[CH:50]=[CH:51][C:52]=1[Cl:53]>C(Cl)Cl>[Cl:46][C:47]1[CH:48]=[C:49]([C:54]2[O:58][C:57]([CH2:59][CH2:60][NH:61][C:12]([C:9]3[NH:10][N:11]=[C:7]([C:4]4[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=4)[CH:8]=3)=[O:14])=[CH:56][CH:55]=2)[CH:50]=[CH:51][C:52]=1[Cl:53]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531Diisopropylethylamine2회HCID 27716315-pyridin-4-yl-4H-pyrazole-3-carboxylic acidHCID 671683442-(5-(3,4-Dichlorophenyl)furan-2-yl)ethanamine hydrochloride

생성물 1

HCID 67174943
N-(2-(5-(3,4-dichlorophenyl)furan-2-yl)ethyl)-3-(pyridin-4-yl)-1H-pyrazole-5-carboxamide
수율 29.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a stirred solution of 5-pyridin-4-yl-4H-pyrazole-3-carboxylic acid (1.78 g, 9.42 mmol) in DCM (10 ml) was added DIPEA (2.46 ml, 14.1 mmol), EDCI (2.71 g, 9.42 mmol) and HOBt (1.91, 14.1 mmol). 2-(5-(3,4-dichlorophenyl)furan-2-yl)-ethanamine hydrochloride (2.75 g, 9.42 mmol) was dissolved in DCM (15 ml) and DIPEA (1.64 ml, 9.42 mmol). The resulting solution was added to the reaction mixture, which was stirred at RT overnight. The reaction mixture was diluted with DCM and washed with saturated aqueous NaHCO3 solution and water. The organic phase was dried over Na2SO4, evaporated and purified by chromatography (CombiFlash, silica column, eluent 0-15% MeOH/DCM). Product containing fractions were collected, evaporated and crystallized from DCM and re-crystallized from 2% MeOH/DCM and heptane. Thus, 1.18 g (29%) of the title compound was obtained. 1H-NMR (400 MHz; d6-DMSO): δ 2.97 (t, 2H), 3.59 (q, 2H), 6.35 (d, 1H), 7.03 (d, 1H), 7.33 (s, 1H), 7.62 (d, 2H), 7.75 (m, 2H), 7.84 (t, 1H), 8.57 (br s, 1H), 8.63 (m, 2H), 13.95 (s, 1H).

후처리

  1. additionThe resulting solution was added to the reaction mixture, which
  2. washwashed with saturated aqueous NaHCO3 solution and water
  3. dry with materialThe organic phase was dried over Na2SO4
  4. customevaporated
  5. custompurified by chromatography (CombiFlash, silica column, eluent 0-15% MeOH/DCM)
  6. additionProduct containing fractions
  7. customwere collected
  8. customevaporated
  9. customcrystallized from DCM
  10. customre-crystallized from 2% MeOH/DCM and heptane

출처 및 근거

ORD 기록
ord-deb3daeeac524b3c92c26b635cf753ea
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08975254B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트