Pyridine → HCID 68891681, 화합물

HRID 2220221노트

반응식

HRID 2220221 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:12][NH:11][C:10]3[CH:13]=[CH:14][C:15]([Cl:17])=[CH:16][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:18]=1.N1C=CC=CC=1.[CH3:25][S:26](Cl)(=[O:28])=[O:27]>ClC(Cl)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:12][N:11]([S:26]([CH3:25])(=[O:28])=[O:27])[C:10]3[CH:13]=[CH:14][C:15]([Cl:17])=[CH:16][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:18]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 68893382HCID 68893382, 화합물

생성물 1

HCID 68891681HCID 68891681, 화합물수율 44.6%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

A solution of 9-Bromo-2-chloro-5,6-dihydro-dibenzo[b,f]azocine (30 mg, 0.09 mmol) (prepared in a manner analogous to that described for Example 1F) in dichloroethane was treated with pyridine (0.02 mL, 0.27 mmol) and methanesulfonyl chloride (0.009 mL, 0.12 mmol). The reaction mixture was stirred at room temperature for two hours then concentrated, diluted with MeOH and filtered. The crude product was purified by preparative reversed-phase HPLC to afford Example 330A (16 mg). HPLC Rt=3.66 min. m/z=398 (M+H+)

후처리

  1. concentrationthen concentrated
  2. additiondiluted with MeOH
  3. filtrationfiltered
  4. customThe crude product was purified by preparative reversed-phase HPLC

출처 및 근거

ORD 기록
ord-8c432488766245c88ce5399ed081dad4
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07417040B2

반응 노트

불러오는 중…