Pyridine → HCID 68891681、化合物

HRID 2220221ノート

反応式

HRID 2220221 の反応式
[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

参加物

5

反応物 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 68893382HCID 68893382、化合物

生成物 1

HCID 68891681HCID 68891681、化合物収率 44.6%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

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+)

後処理

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

出典と根拠

ORDレコード
ord-8c432488766245c88ce5399ed081dad4
出典データセット
uspto-grants-2008_08
特許番号
US07417040B2

反応ノート

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