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

Trifluoroacetic acid → 4-benzenesulfinyl-N-{2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-benzamide

HRID 1177844
노트
인쇄 미리보기

반응식

HRID 1177844 반응식
CCN(C(C)C)C(C)C.[C:10]1([S:16]([C:18]2[CH:26]=[CH:25][C:21]([C:22]([OH:24])=O)=[CH:20][CH:19]=2)=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[NH2:48][CH2:49][C:50]([N:52]1[CH2:57][CH2:56][N:55]([C:58](=[O:69])[C:59]2[CH:64]=[CH:63][CH:62]=[CH:61][C:60]=2[C:65]([F:68])([F:67])[F:66])[CH2:54][CH2:53]1)=[O:51].C(O)(C(F)(F)F)=O>CN(C=O)C.O>[C:10]1([S:16]([C:18]2[CH:19]=[CH:20][C:21]([C:22]([NH:48][CH2:49][C:50](=[O:51])[N:52]3[CH2:53][CH2:54][N:55]([C:58](=[O:69])[C:59]4[CH:64]=[CH:63][CH:62]=[CH:61][C:60]=4[C:65]([F:66])([F:68])[F:67])[CH2:56][CH2:57]3)=[O:24])=[CH:25][CH:26]=2)=[O:17])[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 6422Trifluoroacetic acidHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 3438114-Benzenesulfinyl-benzoic acidHCID 595596292-Amino-1-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone

생성물 1

HCID 25167126
4-benzenesulfinyl-N-{2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-benzamide
수율 51%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

DIPEA (0.084 mL, 0.49 mmol) was added drop wise to 4-benzenesulfinyl-benzoic acid (48 mg, 0.19 mmol) in DMF (4 mL). EDCI (78 mg, 0.41 mmol) and HOBT 26 mg, 0.19 mmol) were added consecutively and 2-amino-1-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone in its TFA salt form (70 mg, 0.16 mmol) was added after a further 10 mins. The resulting mixture was allowed to stir at room temperature overnight. Water was then added and the product was extracted with EtOAc and washed with brine. The organic phase was dried over Na2SO4 and concentrated under reduced pressure to afford a crude product. Purification by column chromatography (using silica gel with a mesh size of 60-120 and 100% EtOAc as eluent) afforded 45 mg (51% yield) of 4-benzenesulfinyl-N-{2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-benzamide. LC-MS purity: 91.93%. 1H NMR (DMSO-D6): δ 8.7 (t, 1H), 8 (m, 3H), 7.8 (m, 6H), 7.5 (m, 3H), 7.2 (m, 1H), 4.2 (d, 2H), 3.6 (m, 6H), 3.1 (m, 2H).

후처리

  1. extractionthe product was extracted with EtOAc
  2. washwashed with brine
  3. dry with materialThe organic phase was dried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customto afford a crude product
  6. customPurification by column chromatography (

출처 및 근거

ORD 기록
ord-2578c01d2e5243ff8ae15ab14638c5d6
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