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

HRID 49295ノート

反応式

HRID 49295 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]=[CH:11][C:12]([N:15]3[CH2:21][CH2:20][CH2:19][N:18]([C:22]4[CH:27]=[CH:26][C:25]([C:28]5[CH:33]=[C:32]([CH3:34])[CH:31]=[C:30]([CH3:35])[CH:29]=5)=[CH:24][N:23]=4)[CH2:17][CH2:16]3)=[N:13][CH:14]=2)[CH:5]=[C:6]([CH3:8])[CH:7]=1.[CH3:36][S:37]([OH:40])(=[O:39])=[O:38]>CO>[CH3:36][S:37]([OH:40])(=[O:39])=[O:38].[CH3:36][S:37]([OH:40])(=[O:39])=[O:38].[CH3:8][C:6]1[CH:5]=[C:4]([C:9]2[CH:10]=[CH:11][C:12]([N:15]3[CH2:21][CH2:20][CH2:19][N:18]([C:22]4[CH:27]=[CH:26][C:25]([C:28]5[CH:33]=[C:32]([CH3:34])[CH:31]=[C:30]([CH3:35])[CH:29]=5)=[CH:24][N:23]=4)[CH2:17][CH2:16]3)=[N:13][CH:14]=2)[CH:3]=[C:2]([CH3:1])[CH:7]=1

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 206349591,4-Bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine

生成物 1

HCID 206349601,4-Bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate収率 90.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1,4-bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (83.0 mg, 0.170 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.37 mL, 0.37 mmol), and the 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 ethanol-diethyl ether-hexane to yield the title compound as colorless needles [melting point: 188.0° C. (decomposed)](101.0 mg, yield: 86%).

後処理

  1. concentrationthe 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 ethanol-diethyl ether-hexane

出典と根拠

ORDレコード
ord-c371c5b1a1fe4433a20455a57571acb6
出典データセット
uspto-grants-2004_03
特許番号
US06706703B2

反応ノート

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