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

HRID 460385ノート

反応式

HRID 460385 の反応式
[O:1]([C:4]1[CH:5]=[C:6]([C:16]2[CH:17]=[CH:18][C:19]([N:22]3[CH2:28][CH2:27][CH2:26][N:25]([C:29]4[CH:34]=[CH:33][C:32]([C:35]5[CH:40]=[C:39]([O:41][CH2:42]C)[C:38]([O:44][CH2:45]C)=[C:37]([O:47][CH2:48]C)[CH:36]=5)=[CH:31][N:30]=4)[CH2:24][CH2:23]3)=[N:20][CH:21]=2)[CH:7]=[C:8]([O:13][CH2:14]C)[C:9]=1[O:10][CH2:11]C)[CH2:2]C.[CH3:50][S:51]([OH:54])(=[O:53])=[O:52]>CO>[CH3:50][S:51]([OH:54])(=[O:53])=[O:52].[CH3:50][S:51]([OH:54])(=[O:53])=[O:52].[CH3:42][O:41][C:39]1[CH:40]=[C:35]([C:32]2[CH:33]=[CH:34][C:29]([N:25]3[CH2:26][CH2:27][CH2:28][N:22]([C:19]4[CH:18]=[CH:17][C:16]([C:6]5[CH:5]=[C:4]([O:1][CH3:2])[C:9]([O:10][CH3:11])=[C:8]([O:13][CH3:14])[CH:7]=5)=[CH:21][N:20]=4)[CH2:23][CH2:24]3)=[N:30][CH:31]=2)[CH:36]=[C:37]([O:47][CH3:48])[C:38]=1[O:44][CH3:45]

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 206349381,4-Bis[5-(3,4,5-triethoxylphenyl)-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収率 94%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1,4-bis[5-(3,4,5-triethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (77 mg, 0.115 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.23 mL, 0.23 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a pale yellow crystalline powder (melting point: 235.0–237.0° C.) (74.0 mg, yield: 94%).

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionEthanol (5.0 mL) was added to the residue
  3. concentrationthe resulting mixture was concentrated under reduced pressure
  4. customThe residue was recrystallized from methanol-diethyl ether

出典と根拠

ORDレコード
ord-534abca251724eb981061ce671bae7b1
出典データセット
uspto-grants-2007_03
特許番号
US07196101B2

反応ノート

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