2-Methylpentane → (R)-1-(Pyridazin-3-ylcarbamoylmethyl)-3-(1-thiophen-2-yl-cycloheptanecarbonyloxy)-1-azonia-bicyclo[2.2.2]octane bromide

HRID 2192310ノート

反応式

HRID 2192310 の反応式
[N:1]12[CH2:8][CH2:7][CH:4]([CH2:5][CH2:6]1)[C@@H:3]([O:9][C:10]([C:12]1([C:19]3[S:20][CH:21]=[CH:22][CH:23]=3)[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)=[O:11])[CH2:2]2.[Br:24][CH2:25][C:26]([NH:28][C:29]1[N:30]=[N:31][CH:32]=[CH:33][CH:34]=1)=[O:27].C(OCC)(=O)C.CCCC(C)C>C(#N)C>[Br-:24].[N:31]1[CH:32]=[CH:33][CH:34]=[C:29]([NH:28][C:26]([CH2:25][N+:1]23[CH2:6][CH2:5][CH:4]([CH2:7][CH2:8]2)[C@@H:3]([O:9][C:10]([C:12]2([C:19]4[S:20][CH:21]=[CH:22][CH:23]=4)[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]2)=[O:11])[CH2:2]3)=[O:27])[N:30]=1

参加物

6

反応物 4

HCID 78922-MethylpentaneHCID 8857Ethyl AcetateHCID 574315532-Bromo-N-pyridazin-3-yl-acetamideHCID 58348375HCID 58348375、化合物

生成物 1

HCID 44516986(R)-1-(Pyridazin-3-ylcarbamoylmethyl)-3-(1-thiophen-2-yl-cycloheptanecarbonyloxy)-1-azonia-bicyclo[2.2.2]octane bromide収率 10.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

1-Thiophen-2-yl-cycloheptanecarboxylic acid (R)-(1-aza-bicyclo[2.2.2]oct-3-yl)ester (Example 5d) (80 mg) and 2-bromo-N-pyridazin-3-yl-acetamide (Example 5e) (52 mg) were dissolved in acetonitrile (3 mL) and stirred overnight. Ethyl acetate (9 mL) and isohexane (4 mL) were added and stirred overnight. The resulting crystals were filtered off and then triturated with ethyl acetate to afford the titled compound (14 mg).

後処理

  1. stirringstirred overnight
  2. filtrationThe resulting crystals were filtered off
  3. customtriturated with ethyl acetate

出典と根拠

ORDレコード
ord-c6bfc223041e4668b782e43772e947d5
出典データセット
uspto-grants-2012_12
特許番号
US08329729B2

反応ノート

読み込み中…