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

p-Bromobenzenesulfonyl chloride → Methyl 5-{[[(4-bromophenyl)sulfonyl](hexyl)amino]methyl}-2-fluorobenzoate

HRID 551991
노트
인쇄 미리보기

반응식

HRID 551991 반응식
[F:1][C:2]1[CH:11]=[CH:10][C:9]([CH2:12][NH:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[Br:20][C:21]1[CH:26]=[CH:25][C:24]([S:27](Cl)(=[O:29])=[O:28])=[CH:23][CH:22]=1.C([O-])(O)=O.[Na+]>C(Cl)Cl>[Br:20][C:21]1[CH:26]=[CH:25][C:24]([S:27]([N:13]([CH2:12][C:9]2[CH:10]=[CH:11][C:2]([F:1])=[C:3]([CH:8]=2)[C:4]([O:6][CH3:7])=[O:5])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])(=[O:29])=[O:28])=[CH:23][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7396p-Bromobenzenesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 57554492Methyl 2-fluoro-5-[(hexylamino)methyl]benzoate

생성물 1

HCID 57554548Methyl 5-{[[(4-bromophenyl)sulfonyl](hexyl)amino]methyl}-2-fluorobenzoate수율 25%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of methyl 2-fluoro-5-[(hexylamino)methyl]benzoate in DCM (13 mL) were added 4-bromobenzenesulfonyl chloride (200 mg; 0.79 mmol) and TEA (0.13 mL; 0.94 mmol). The reaction mixture was stirred at room temperature for 2 hours under N2 atmosphere. The mixture was poured into a saturated solution of NaHCO3 and extracted with DCM (2×100 mL). The combined organic layers were then washed with a saturated solution of NH4Cl (150 mL) and with brine (150 mL), dried over magnesium sulfate, filtrated and the solvent was removed under reduced pressure. Purification by flash chromatography on silica gel (c-Hex/EtOAc, 95:5) gave 96 mg (25%) of the title compound as a colorless oil. HPLC, Rt: 5.13 min (purity=99.1%). LC/MS: M+(ESI): 486.23; 1H NMR (CDCl3) δ: 7.78 (m, 1H), 7.72 (m, 4H), 7.55 (m, 1H), 7.12 (m, 1H), 4.31 (s, 2H), 3.93 (s, 3H), 3.09 (t, J=7.5 Hz, 2H), 1.85 to 1.05 (m, 8H), 0.81 (t, J=6.9 Hz, 3H).

후처리

  1. extractionextracted with DCM (2×100 mL)
  2. washThe combined organic layers were then washed with a saturated solution of NH4Cl (150 mL) and with brine (150 mL)
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltrated
  5. customthe solvent was removed under reduced pressure
  6. customPurification by flash chromatography on silica gel (c-Hex/EtOAc, 95:5)

출처 및 근거

ORD 기록
ord-c4730ff378384285a1448165416c3886
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07947851B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트