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

HRID 49295노트

반응식

HRID 49295 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c371c5b1a1fe4433a20455a57571acb6
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706703B2

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