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

Dichloromethane → (2-Benzyl-6-methoxy-benzo[b]thiophen-3-yl)-(4-methoxy-phenyl)-methanone

HRID 1873123
노트
인쇄 미리보기

반응식

HRID 1873123 반응식
[Sn](Cl)(Cl)(Cl)Cl.[CH2:6]([C:13]1[S:17][C:16]2[CH:18]=[C:19]([O:22][CH3:23])[CH:20]=[CH:21][C:15]=2[CH:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[C:24](Cl)(=[O:33])[C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=1.ClCCl>O>[CH2:6]([C:13]1[S:17][C:16]2[CH:18]=[C:19]([O:22][CH3:23])[CH:20]=[CH:21][C:15]=2[C:14]=1[C:24]([C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=1)=[O:33])[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 7477p-Anisoyl chlorideHCID 24287Tin tetrachlorideHCID 186877862-Benzyl-6-methoxy-benzo[b]thiophene

생성물 1

HCID 15481275(2-Benzyl-6-methoxy-benzo[b]thiophen-3-yl)-(4-methoxy-phenyl)-methanone수율 58.5%

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

Tin tetrachloride (2.0 mL, 17.09 mmol) was added dropwise over a 10 minute period to a stirred, -78° C. solution of 2-benzyl-6-methoxy-benzo[b]thiophene (2.71 g, 10.65 mmol), anisoyl chloride (1.93 g, 11.29 mmol) and dichloromethane (41 mL) under a dry nitrogen atmosphere. After 1 hours at -78° C., the reaction mixture was slowly warmed to room temperature and stirred for 16 h period. The reaction mixture was added to water and extracted with ether. The ether phase was washed with brine and silica gel was added to it. The solvent was removed and the adsorbate was flash chromatographed (eluent: 9:1 petroleum ether: ethyl acetate) to provide the title compound as a white solid (2.42 g, 58%): mp 110-112° C.: NMR (CDCl3); δ 7.84 (d, J=9 Hz, 2H), 7.31-7.18 (m, 7H), 7.92 (d, J=9 Hz, 2H), 6.97 (dd, J=9, 2 Hz, 1H), 4.17 (s, 2H), 3.88 (s, 3H), 3.883 (s, 3H); MS (FAB+): 389 (80%, M+H); Anal. Calc. for C24H20O3S: C, 74.20, H, 5.19, N, 0.00. Found: C, 74.94, H, 5.10, N, 0.03.

후처리

  1. extractionextracted with ether
  2. washThe ether phase was washed with brine and silica gel
  3. additionwas added to it
  4. customThe solvent was removed
  5. customchromatographed (eluent: 9:1 petroleum ether: ethyl acetate)

출처 및 근거

ORD 기록
ord-575c11a0c03446e089de3f29cf9e07d0
출처 데이터셋
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06110962

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트