Methanesulfonic Acid → 1,4-Bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate

HRID 49298

反応式

HRID 49298 の反応式
[O:1]([C:3]1[CH:4]=[C:5]([C:13]2[CH:14]=[CH:15][C:16]([N:19]3[CH2:25][CH2:24][CH2:23][N:22]([C:26]4[CH:31]=[CH:30][C:29]([C:32]5[CH:37]=[C:36]([O:38][CH3:39])[C:35]([O:40][CH3:41])=[C:34]([O:42][CH3:43])[CH:33]=5)=[CH:28][N:27]=4)[CH2:21][CH2:20]3)=[N:17][CH:18]=2)[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10])[CH3:2].[CH3:44][S:45]([OH:48])(=[O:47])=[O:46]>C(O)C.C(Cl)(Cl)Cl>[CH3:44][S:45]([OH:48])(=[O:47])=[O:46].[CH3:44][S:45]([OH:48])(=[O:47])=[O:46].[CH3:39][O:38][C:36]1[CH:37]=[C:32]([C:29]2[CH:30]=[CH:31][C:26]([N:22]3[CH2:23][CH2:24][CH2:25][N:19]([C:16]4[CH:15]=[CH:14][C:13]([C:5]5[CH:4]=[C:3]([O:1][CH3:2])[C:8]([O:9][CH3:10])=[C:7]([O:11][CH3:12])[CH:6]=5)=[CH:18][N:17]=4)[CH2:20][CH2:21]3)=[N:27][CH:28]=2)[CH:33]=[C:34]([O:42][CH3:43])[C:35]=1[O:40][CH3:41]

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 206349241,4-Bis[5-(3,4,5-trimethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine

生成物 1

HCID 206349231,4-Bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate

試薬・触媒・溶媒 1

HCID 21889567Chloroform ethanol溶媒

実験手順

To a solution of 1,4-bis[5-(3,4,5-trimethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (72.4 g, 0.120 mol) in ethanol-chloroform (1:3, 600 mL) was added methanesulfonic acid (24.9 g, 0.258 mol), and the reaction mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a slightly yellow crystalline powder (melting point: 204.0-206.0° C.) (88.2 g, yield: 92%).

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customThe residue was recrystallized from methanol-diethyl ether

出典と根拠

ORDレコード
ord-780fc6867ddc4e848145f2500a1a1acc
出典データセット
uspto-grants-2004_03
特許番号
US06706703B2

関連ノート

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