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

1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → ethyl 3-(7-{5-[6-[(1-methylethyl)oxy]-5-(trifluoromethyl)-3-pyridinyl]-1,2,4-oxadiazol-3-yl}-1H-indol-3-yl)propanoate

HRID 1512750
노트
인쇄 미리보기

반응식

HRID 1512750 반응식
CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[CH3:22][CH:23]([O:25][C:26]1[N:31]=[CH:30][C:29]([C:32]([OH:34])=O)=[CH:28][C:27]=1[C:35]([F:38])([F:37])[F:36])[CH3:24].O[NH:40]/[C:41](=[N:58]\[H])/[C:42]1[CH:43]=[CH:44][CH:45]=[C:46]2[C:50]=1[NH:49][CH:48]=[C:47]2[CH2:51][CH2:52][C:53]([O:55][CH2:56][CH3:57])=[O:54].CCCC[N+](CCCC)(CCCC)CCCC.[F-]>C1COCC1>[CH3:24][CH:23]([O:25][C:26]1[N:31]=[CH:30][C:29]([C:32]2[O:34][N:58]=[C:41]([C:42]3[CH:43]=[CH:44][CH:45]=[C:46]4[C:50]=3[NH:49][CH:48]=[C:47]4[CH2:51][CH2:52][C:53]([O:55][CH2:56][CH3:57])=[O:54])[N:40]=2)=[CH:28][C:27]=1[C:35]([F:38])([F:37])[F:36])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 2724141Tetrabutylammonium FluorideHCID 670252766-[(1-Methylethyl)oxy]-5-(trifluoromethyl)-3-pyridinecarboxylic acidHCID 178506492HCID 178506492, 화합물

생성물 1

HCID 59146041
ethyl 3-(7-{5-[6-[(1-methylethyl)oxy]-5-(trifluoromethyl)-3-pyridinyl]-1,2,4-oxadiazol-3-yl}-1H-indol-3-yl)propanoate
수율 42.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

EDCI (153 mg) and HOBT (132 mg) were added to a solution of 6-[(1-methylethyl)oxy]-5-(trifluoromethyl)-3-pyridinecarboxylic acid (100 mg) in THF (2.5 mL). The mixture was stirred at room temperature for 0.5 hour, followed by addition of ethyl 3-{7-[(Z)-(hydroxyamino)(imino)methyl]-1H-indol-3-yl}propanoate (D35) (165 mg) in THF (2.5 mL). The resulting mixture was stirred at room temperature for 1 hour, followed by addition of TBAF (418 mg). The reaction vessel was sealed and the reaction mixture was stirred at 120° C. in the microwave for 1.5 h. THF was removed. The residue was dissolved in EtOAc. The organic solution was washed with saturated aqueous sodium bicarbonate solution. The organic solution was dried over anhydrous sodium sulfate. The dried solution was concentrated. The residue was purified by column chromatography to afford ethyl 3-(7-{5-[6-[(1-methylethyl)oxy]-5-(trifluoromethyl)-3-pyridinyl]-1,2,4-oxadiazol-3-yl}-1H-indol-3-yl)propanoate (D37) (83 mg) as a white solid. δH (CDCl3, 400 MHz): 1.24 (3H, t), 1.45 (6H, d), 2.74 (2H, t), 3.17 (2H, t), 4.15 (2H, q), 5.58 (1H, m), 7.19 (1H, d), 7.29 (1H, d), 7.82 (1H, d), 8.12 (1H, dd), 8.64 (1H, d), 9.17 (1H, d), 9.55 (1H, s); MS (ES): C24H23F3N4O4 requires 488; found 489.2 (M+H+).

후처리

  1. stirringThe resulting mixture was stirred at room temperature for 1 hour
  2. customThe reaction vessel was sealed
  3. stirringthe reaction mixture was stirred at 120° C. in the microwave for 1.5 h
  4. customTHF was removed
  5. dissolutionThe residue was dissolved in EtOAc
  6. washThe organic solution was washed with saturated aqueous sodium bicarbonate solution
  7. dry with materialThe organic solution was dried over anhydrous sodium sulfate
  8. concentrationThe dried solution was concentrated
  9. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-e56b8e25a59340458f1d6d33bf07edf3
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08217028B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트