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

N,N-Dimethylglycine → 1-[4-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)piperidino]-2-(dimethylamino)-1-ethanone

HRID 748806
노트
인쇄 미리보기

반응식

HRID 748806 반응식
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([C:12]2([C:18]3[CH:23]=[C:22]([F:24])[CH:21]=[CH:20][C:19]=3[F:25])[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)(=[O:11])=[O:10])=[CH:5][CH:4]=1.[CH3:26][N:27]([CH3:32])[CH2:28][C:29](O)=[O:30].CN1CCOCC1.Cl.C(N=C=NCCCN(C)C)C.C(=O)(O)[O-].[Na+]>ClCCl.C(OC(C)C)(C)C>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([C:12]2([C:18]3[CH:23]=[C:22]([F:24])[CH:21]=[CH:20][C:19]=3[F:25])[CH2:17][CH2:16][N:15]([C:29](=[O:30])[CH2:28][N:27]([CH3:32])[CH3:26])[CH2:14][CH2:13]2)(=[O:10])=[O:11])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 673N,N-DimethylglycineHCID 79724-MethylmorpholineHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 692029464-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)piperidine Hydrochloride

생성물 1

HCID 59750866
1-[4-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)piperidino]-2-(dimethylamino)-1-ethanone
수율 62%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 7914Diisopropyl Ether용매

실험 절차

The 4-[(4-chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)piperidine hydrochloride (100 mg, 0.245 mmol) obtained in Example 260, N,N-dimethylglycine (40 mg, 0.39 mmol) and N-methylmorpholine (0.142 ml, 1.29 mmol) were dissolved in dichloromethane (5 ml), followed by the addition of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (80 mg, 0.42 mmol) at room temperature. After stirring at room temperature for 14 hours, a saturated aqueous solution (0.5 ml) of sodium bicarbonate was added. The residue obtained by concentrating the reaction mixture under reduced pressure was subjected to flash silica gel chromatography, and the fraction obtained from the dichloromethane:methanol=30:1 eluate was concentrated under reduced pressure to give a white solid. The resulting solid was washed with diisopropyl ether, whereby the title compound (70 mg, 0.15 mmol, 62%) was obtained as a white powder.

후처리

  1. customThe residue obtained
  2. concentrationby concentrating the reaction mixture under reduced pressure
  3. customthe fraction obtained from the dichloromethane
  4. concentrationmethanol=30:1 eluate was concentrated under reduced pressure
  5. customto give a white solid

출처 및 근거

ORD 기록
ord-f44f9405391c42c594c0be2b9d1b5c1c
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07399775B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트