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

1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 2,4-Difluoro-biphenyl-4-carboxylic acid {2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-amide

HRID 1177891
노트
인쇄 미리보기

반응식

HRID 1177891 반응식
CCN(C(C)C)C(C)C.[F:10][C:11]1[CH2:16][C:15]([F:20])([C:17]([OH:19])=O)[CH:14]=[CH:13][C:12]=1[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.[NH2:49][CH2:50][C:51]([N:53]1[CH2:58][CH2:57][N:56]([C:59](=[O:70])[C:60]2[CH:65]=[CH:64][CH:63]=[CH:62][C:61]=2[C:66]([F:69])([F:68])[F:67])[CH2:55][CH2:54]1)=[O:52]>CN(C=O)C.C(OCC)(=O)C.O>[O:52]=[C:51]([N:53]1[CH2:54][CH2:55][N:56]([C:59](=[O:70])[C:60]2[CH:65]=[CH:64][CH:63]=[CH:62][C:61]=2[C:66]([F:69])([F:68])[F:67])[CH2:57][CH2:58]1)[CH2:50][NH:49][C:17]([C:15]1([F:20])[CH:14]=[CH:13][C:12]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:11]([F:10])[CH2:16]1)=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 669531782-Amino-1-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone hydrochlorideHCID 669533272,4-Difluoro-biphenyl-4-carboxylic acid

생성물 1

HCID 86634089
2,4-Difluoro-biphenyl-4-carboxylic acid {2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-amide
수율 50.8%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

DIPEA (83 mg, 0.11 mL, 0.21 mmol) was added to a stirred solution of 2,4-difluoro-biphenyl-4-carboxylic acid (50 mg, 0.21 mmol) in DMF (1 mL). HOBT (35 mg, 0.25 mmol) and EDCI (50 mg, 0.25 mmol) were then added at room temperature. After 2 minutes 2-amino-1-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone hydrochloride salt (90 mg, 0.25 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added and then extrated with ethyl acetate. The organic layer was washed with brine and dried over Na2SO4 and concentrated under reduced pressure to afford 56.9 mg (50.35%) of 2,4-difluoro-biphenyl-4-carboxylic acid {2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-amide. LCMS Purity: 95.42%. 1H NMR (DMSO-d6): δ 8.2-7.94 (d, 2H), 7.88-7.74 (m, 2H), 7.74-7.6 (m, 4H), 7.6-7.5 (m, 1H), 7.46-7.34 (m, 1H), 7.3-7.2 (m, 1H), 4.3-4.1 (m, 2H), 3.8-3.4 (m, 6H), 3.2-3.0 (m, 2H).

후처리

  1. washThe organic layer was washed with brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1e79d29a93a3425e95b53c9ba16e7ff2
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07842696B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트