Pyridine → HCID 69196441, 화합물

HRID 2220220노트

반응식

HRID 2220220 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.[CH:25]1([C:28](Cl)=[O:29])[CH2:27][CH2:26]1>ClC(Cl)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:12][N:11]([C:28]([CH:25]3[CH2:27][CH2:26]3)=[O:29])[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 77637Cyclopropanecarbonyl chlorideHCID 68893382HCID 68893382, 화합물

생성물 1

HCID 69196441HCID 69196441, 화합물수율 85.8%

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 cyclopropanecarbonyl chloride (0.011 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 326A (30 mg, 82%). HPLC Rt=4.05 min. m/z=388 (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-5b86ed301a7341349af4570d5f6acd8f
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07417040B2

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