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

HCID 86585865, 화합물 → HCID 86585866, 화합물

HRID 1246842
노트
인쇄 미리보기

반응식

HRID 1246842 반응식
[CH:1]([C:4]1[C:9]([C:10]([F:13])([F:12])[F:11])=[C:8]([S:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:7]=[CH:6][C:5]=1[C:21]1[CH:26]=[CH:25][N+:24]([O-])=[CH:23][CH:22]=1)([CH3:3])[CH3:2]>O=P(Cl)(Cl)Cl>[CH:1]([C:4]1[C:9]([C:10]([F:13])([F:11])[F:12])=[C:8]([S:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:7]=[CH:6][C:5]=1[C:21]1[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=1)([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 86585865HCID 86585865, 화합물

생성물 1

HCID 86585866HCID 86585866, 화합물수율 89.6%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

Then, 2-chloro-4-(4-(2-isopropyl-phenylsulfanyl-3-trifluoromethyl-phenyl)-pyridine 76 was prepared as follows. Compound 75 (3.19 g, 8.19 mmol) was treated with POCl3 (50 mL) at 100° C. for 10 hours. The reaction mixture was concentrated on a rotovap, and the residue was treated with crushed ice (20 g). Water (100 mL) was added, the aqueous solution was then extracted with ethyl acetate (2×100 mL). The combined organic layers were washed with brine (3×100 mL), dried over MgSO4, filtered and concentrated. The crude product was purified by chromatography to give the title compound 76 as a brown oil (2.74 g, 82%). 1H-NMR (CDCl3, 400 MHz) δ 1.19 (d, J=6.8 Hz, 6H), 3.51 (heptet, J=6.8 Hz, 1H), 6.91 (d, J=8.5 Hz, 1H), 7.25–7.28 (m, 1H), 7.37 (dd, J=1.7 Hz, 5.1 Hz, 1H), 7.45–7.52 (m, 5H), 7.87 (d, J=2.0 Hz, 1H), 8.43 (d, J=5.4 Hz, 1H). MS (DCI) m/z 408, 409, 410 (M+H)+.

후처리

  1. customThen, 2-chloro-4-(4-(2-isopropyl-phenylsulfanyl-3-trifluoromethyl-phenyl)-pyridine 76 was prepared
  2. concentrationThe reaction mixture was concentrated on a rotovap
  3. additionthe residue was treated with crushed ice (20 g)
  4. additionWater (100 mL) was added
  5. extractionthe aqueous solution was then extracted with ethyl acetate (2×100 mL)
  6. washThe combined organic layers were washed with brine (3×100 mL)
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe crude product was purified by chromatography

출처 및 근거

ORD 기록
ord-d2681bdeddcd40478bcc829427297c18
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07129247B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트